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In the crystal structure of the title compound, [ZnCl2{(C6H5)3PO}2]·2THF (THF is tetra­hydro­furan, C4H8O), the ZnII ion is four-coordinated by two Cl atoms and two O atoms in a distorted tetrahedral geometry. Additionally, two solvent THF mol­ecules occupy the open space in the unit cell, not bonding to the Zn atom. The Zn-Cl distances are 2.2108 (6) and 2.2165 (6) Å, and the Zn-O distances are 1.9851 (15) and 1.9751 (15) Å. Within the tetrahedral coordination sphere around the central Zn atom, the bond angles are O1-Zn-O2 98.16 (6)° and Cl1-Zn-Cl2 120.55 (2)°; the four Cl-Zn-O bond angles range from 107.43 (4) to 110.55 (4)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801015318/cv6052sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801015318/cv6052Isup2.hkl
Contains datablock I

CCDC reference: 175343

Key indicators

  • Single-crystal X-ray study
  • T = 123 K
  • Mean [sigma](C-C) = 0.003 Å
  • Disorder in solvent or counterion
  • R factor = 0.033
  • wR factor = 0.087
  • Data-to-parameter ratio = 11.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 23.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

Recently Mayer (1998) introduced the bond-strength concept, i.e. the importance of the thermodynamics of broken and formed bonds. Because of the importance of phosphine ligands in organometallic chemistry we decided to investigate a series of metal complexes with triphenylphosphine and triphenylphosphine oxide ligands structurally and computationally. In the course of our investigation of the coordination strength of triphenylphosphine and triphenylphosphine oxide, we have been able to redetermine the crystal structure of the title complex, (I). It has originally been reported without solvent molecules by Rose et al. (1980) and Kosky et al. (1982). Structures of the type [M{(C6H5)3PO}2Cl2] with M = CoII (Mangion, 1976) and M = CuII (Bertrand et al., 1971) had previously been investigated. Studies on the IR spectra of compounds with M = ZnII by Deacon & Green (1968, 1969), as well as the thermochemistry of M = ZnII, CdII, HgII investigated by Jorge et al. (1978) gives us valuable information whether the calculated bond strength are in good agreement with experimental data.

As can be seen in Fig. 1, the ZnII ion in the title compound has a slightly distorted tetrahedral coordination, where the metal is ligated by two O atoms and two Cl atoms. Compared to the C2-symmetrical structure, (II), reported by Rose et al. (1980), (I) shows no point symmetry, a result of the two solvent molecules present in the crystal. The THF molecules occupy the open space in the structure and are not bound to the central atom. Their incorporation also results in a slight flatening of the molecule in (I), as can seen by the larger Cl1—Zn—Cl2 angle of 120.55 (2)° and O1—Zn—O2 angle of 98.16 (6)° compared to 116.3 and 96.8° in (II). The biggest change in bond angles can be seen in the decrease of the Zn—O—P angle from 153.4° in (II) to 139.20 (9) and 141.01 (9)° in (I), whereas the effect on the O—P—C angles is negligible.

Furthermore the Cl—Zn—O—P torsion angles changed from -38.9° in (II) to -8.3 (2)° and -8.8 (2)° in (I). A comparison of the corresponding Zn—O—P—C torsion angles indicates a rotation of the triphenylphosphine group of about 20° in the present compound induced by the thf molecules in the structure, e.g. 78.3 (2) and 76.0 (2)° in (I) versus 54.7° in the earlier structure (II).

Experimental top

The title compound was prepared by adding oxygen to a suspension of Ni[P(C6H5)3]4 and two equivalents of ZnCl2 in toluene at 333 K. After filtration and removal of the solvent, colorless crystals were obtained by slowly cooling a saturated solution in tetrahydrofuran from 313 K to room temperature. NMR data validate the presence of two THF molecules in the crystal. All H atoms were located in the difference Fourier maps and refined freely except those located at the disordered THF solvent molecule. They were calculated in ideal positions and refined as a riding model.

Refinement top

Straight forward after integration with the program NPROCESS, source: Nonius (2000b).

Computing details top

Data collection: Kappa-CCD Control Software (Nonius, 2000); cell refinement: DENZO (Nonius, 2000); data reduction: DENZO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1998); molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: PLATON.

Figures top
[Figure 1] Fig. 1. View of the title compound with the appropriate atom-numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. The H atoms and THF molecules have been omitted for clarity.
Dichlorobis(triphenylphosphine oxide)zinc(II) top
Crystal data top
[ZnCl2(C18H15OP)2]·2C4H8OZ = 2
Mr = 837.04F(000) = 872
Triclinic, P1Dx = 1.386 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.6758 (1) ÅCell parameters from 7093 reflections
b = 12.9704 (1) Åθ = 1.5–25.4°
c = 15.2874 (2) ŵ = 0.87 mm1
α = 110.2721 (4)°T = 123 K
β = 109.8102 (5)°Fragment, colorless
γ = 92.8572 (4)°0.69 × 0.61 × 0.45 mm
V = 2006.16 (4) Å3
Data collection top
Nonius κ-CCD
diffractometer
7358 independent reflections
Radiation source: NONIUS FR 591 rotating anode6793 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Detector resolution: 18 # 9 for binned mode pixels mm-1θmax = 25.4°, θmin = 1.5°
ϕ and ω–rotation scansh = 1414
Absorption correction: multi-scan
applied during the scaling procedure (Nonius, 2000)
k = 1515
Tmin = 0.559, Tmax = 0.677l = 1818
30256 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: difference Fourier map
wR(F2) = 0.087H atoms treated by a mixture of independent and constrained refinement
S = 1.05Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo2) + (0.0454P)2 + 1.6738P]
where P = (Fo2 + 2Fc2)/3
7357 reflections(Δ/σ)max = 0.001
640 parametersΔρmax = 0.54 e Å3
0 restraintsΔρmin = 0.45 e Å3
Crystal data top
[ZnCl2(C18H15OP)2]·2C4H8Oγ = 92.8572 (4)°
Mr = 837.04V = 2006.16 (4) Å3
Triclinic, P1Z = 2
a = 11.6758 (1) ÅMo Kα radiation
b = 12.9704 (1) ŵ = 0.87 mm1
c = 15.2874 (2) ÅT = 123 K
α = 110.2721 (4)°0.69 × 0.61 × 0.45 mm
β = 109.8102 (5)°
Data collection top
Nonius κ-CCD
diffractometer
7358 independent reflections
Absorption correction: multi-scan
applied during the scaling procedure (Nonius, 2000)
6793 reflections with I > 2σ(I)
Tmin = 0.559, Tmax = 0.677Rint = 0.046
30256 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.087H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.54 e Å3
7357 reflectionsΔρmin = 0.45 e Å3
640 parameters
Special details top

Experimental. Diffractometer operator E. Herdtweck scanspeed 2 x 30 s per film repetition 1 713 films measured in 5 data sets set 1: phi-scan with delta_phi = 1.0 set 2 to set 5 omega-scan with delta_omega = 1.0

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R_factor_obs 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
xyzUiso*/UeqOcc. (<1)
Zn0.64187 (2)0.32970 (2)0.24670 (2)0.0154 (1)
Cl10.66504 (5)0.47594 (4)0.38414 (4)0.0255 (2)
Cl20.47745 (4)0.28918 (4)0.10581 (4)0.0214 (1)
P10.84041 (4)0.32142 (4)0.13636 (4)0.0146 (1)
P20.68851 (4)0.16018 (4)0.36648 (4)0.0157 (1)
O10.65444 (12)0.19270 (11)0.27690 (10)0.0185 (4)
O20.79611 (12)0.34168 (11)0.22146 (10)0.0180 (4)
C110.82066 (18)0.43194 (15)0.09049 (14)0.0166 (5)
C120.70275 (19)0.45743 (18)0.05869 (16)0.0222 (6)
C130.6859 (2)0.54767 (18)0.03016 (16)0.0245 (6)
C140.7857 (2)0.61278 (17)0.03346 (15)0.0226 (6)
C150.9021 (2)0.58757 (17)0.06404 (16)0.0227 (6)
C160.92004 (19)0.49687 (17)0.09227 (15)0.0189 (6)
C210.76057 (17)0.19142 (16)0.03341 (15)0.0179 (5)
C220.70686 (19)0.10799 (17)0.05286 (17)0.0227 (6)
C230.6497 (2)0.00447 (18)0.02417 (18)0.0278 (7)
C240.6478 (2)0.01629 (18)0.11965 (17)0.0279 (7)
C250.7006 (2)0.06604 (19)0.13941 (17)0.0283 (7)
C260.7563 (2)0.17075 (18)0.06312 (16)0.0235 (6)
C311.00262 (17)0.31794 (16)0.18127 (15)0.0169 (5)
C321.05906 (19)0.26065 (17)0.11654 (16)0.0214 (6)
C331.1848 (2)0.26193 (19)0.15425 (17)0.0253 (7)
C341.2546 (2)0.3188 (2)0.25582 (18)0.0284 (7)
C351.1991 (2)0.37590 (19)0.32026 (17)0.0278 (7)
C361.07318 (19)0.37583 (17)0.28316 (16)0.0214 (6)
C410.56767 (18)0.16674 (17)0.41458 (14)0.0181 (6)
C420.5380 (2)0.27083 (18)0.45600 (16)0.0243 (6)
C430.4379 (2)0.2775 (2)0.48447 (17)0.0307 (7)
C440.3668 (2)0.1817 (2)0.47232 (18)0.0336 (8)
C450.3964 (2)0.0783 (2)0.43263 (18)0.0332 (8)
C460.4969 (2)0.07064 (19)0.40345 (16)0.0248 (6)
C510.82845 (18)0.24631 (16)0.46662 (15)0.0190 (6)
C520.9171 (2)0.29124 (18)0.44121 (17)0.0247 (6)
C531.0289 (2)0.3546 (2)0.51544 (18)0.0300 (7)
C541.0529 (2)0.37221 (18)0.61517 (17)0.0276 (7)
C550.9651 (2)0.32747 (18)0.64061 (16)0.0269 (7)
C560.8523 (2)0.26508 (17)0.56714 (15)0.0230 (6)
C610.71345 (18)0.01872 (16)0.32849 (15)0.0174 (5)
C620.7861 (2)0.02154 (18)0.39793 (17)0.0242 (6)
C630.8035 (2)0.13109 (19)0.36552 (18)0.0279 (7)
C640.7497 (2)0.20021 (18)0.26495 (18)0.0280 (7)
C650.6774 (2)0.16084 (18)0.19563 (18)0.0284 (7)
C660.6592 (2)0.05100 (17)0.22732 (16)0.0232 (6)
O810.0057 (2)0.86988 (15)0.12813 (14)0.0484 (7)
C82A0.0169 (4)0.9761 (3)0.1251 (3)0.0693 (13)0.531 (15)
C83A0.0487 (13)1.0600 (5)0.2347 (5)0.054 (3)0.531 (15)
C84A0.0433 (3)0.9979 (3)0.2937 (2)0.0539 (10)0.531 (15)
C850.0405 (3)0.8799 (2)0.2300 (2)0.0400 (9)
C84B0.0433 (3)0.9979 (3)0.2937 (2)0.0539 (10)0.469 (15)
C82B0.0169 (4)0.9761 (3)0.1251 (3)0.0693 (13)0.469 (15)
C83B0.0284 (10)1.0467 (6)0.2213 (5)0.038 (2)0.469 (15)
O710.3094 (2)0.73622 (17)0.26140 (16)0.0582 (8)
C720.2621 (2)0.6180 (3)0.2162 (2)0.0440 (9)
C730.3728 (2)0.5649 (2)0.24294 (19)0.0334 (7)
C740.4722 (3)0.6429 (2)0.2426 (2)0.0407 (8)
C750.4328 (3)0.7535 (2)0.2698 (3)0.0552 (10)
H1210.638 (2)0.411 (2)0.0580 (18)0.029 (6)*
H1310.605 (2)0.5625 (19)0.0066 (17)0.023 (6)*
H1410.774 (2)0.673 (2)0.0143 (18)0.025 (6)*
H1510.969 (2)0.634 (2)0.0702 (19)0.033 (7)*
H1610.998 (2)0.4789 (18)0.1110 (16)0.018 (5)*
H2210.707 (2)0.121 (2)0.118 (2)0.036 (7)*
H2310.612 (2)0.049 (2)0.012 (2)0.034 (7)*
H2410.6083 (19)0.0855 (18)0.1736 (17)0.014 (5)*
H2510.700 (2)0.054 (2)0.205 (2)0.032 (7)*
H2610.790 (2)0.225 (2)0.0743 (18)0.028 (6)*
H3211.012 (2)0.2212 (19)0.0469 (18)0.020 (6)*
H3311.222 (2)0.224 (2)0.1140 (19)0.027 (6)*
H3411.343 (2)0.3189 (19)0.2793 (18)0.024 (6)*
H3511.249 (2)0.418 (2)0.392 (2)0.031 (7)*
H3611.036 (2)0.4167 (19)0.3275 (18)0.021 (6)*
H4210.587 (2)0.334 (2)0.4651 (17)0.023 (6)*
H4310.422 (2)0.344 (2)0.511 (2)0.033 (7)*
H4410.299 (2)0.186 (2)0.4911 (19)0.035 (7)*
H4510.347 (3)0.011 (2)0.425 (2)0.045 (8)*
H4610.519 (2)0.003 (2)0.3783 (18)0.028 (6)*
H5210.901 (2)0.276 (2)0.372 (2)0.039 (7)*
H5311.090 (2)0.386 (2)0.4983 (19)0.032 (7)*
H5411.123 (2)0.414 (2)0.6678 (19)0.026 (6)*
H5510.979 (2)0.340 (2)0.709 (2)0.029 (6)*
H5610.788 (2)0.234 (2)0.5829 (19)0.031 (6)*
H6210.821 (2)0.021 (2)0.463 (2)0.024 (6)*
H6310.852 (2)0.160 (2)0.410 (2)0.037 (7)*
H6410.761 (2)0.273 (2)0.2450 (19)0.033 (7)*
H6510.637 (2)0.208 (2)0.128 (2)0.037 (7)*
H6610.612 (2)0.025 (2)0.1793 (19)0.027 (6)*
H8210.105300.981900.098500.0830*0.531 (15)
H8410.032101.003700.309500.0650*0.531 (15)
H8420.117001.025200.357600.0650*0.531 (15)
H8510.124900.862400.248800.0480*
H8520.014100.827200.239500.0480*
H8220.023100.990200.081600.0830*0.531 (15)
H8310.135801.088800.248400.0650*0.531 (15)
H8320.005501.123900.248800.0650*0.531 (15)
H8230.091200.970400.066600.0830*0.469 (15)
H8240.057101.009100.119300.0830*0.469 (15)
H8330.116201.040700.214300.0450*0.469 (15)
H8340.008201.126200.243000.0450*0.469 (15)
H8430.129701.039900.331400.0650*0.469 (15)
H8440.004300.999900.342400.0650*0.469 (15)
H7210.223 (3)0.597 (3)0.146 (3)0.053 (9)*
H7220.200 (3)0.607 (3)0.243 (3)0.075 (11)*
H7310.362 (3)0.487 (3)0.195 (2)0.056 (9)*
H7320.392 (2)0.562 (2)0.314 (2)0.038 (7)*
H7410.551 (3)0.644 (3)0.290 (2)0.052 (9)*
H7420.472 (3)0.622 (3)0.176 (3)0.053 (9)*
H7510.490 (4)0.807 (4)0.338 (3)0.096 (13)*
H7520.439 (3)0.795 (3)0.228 (3)0.074 (11)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.0171 (1)0.0153 (1)0.0144 (1)0.0033 (1)0.0065 (1)0.0059 (1)
Cl10.0316 (3)0.0195 (2)0.0219 (3)0.0056 (2)0.0123 (2)0.0019 (2)
Cl20.0187 (2)0.0225 (2)0.0207 (2)0.0022 (2)0.0028 (2)0.0103 (2)
P10.0155 (2)0.0151 (2)0.0139 (2)0.0025 (2)0.0058 (2)0.0062 (2)
P20.0197 (2)0.0150 (2)0.0135 (2)0.0036 (2)0.0070 (2)0.0061 (2)
O10.0245 (7)0.0168 (7)0.0154 (7)0.0037 (5)0.0076 (6)0.0076 (6)
O20.0190 (7)0.0213 (7)0.0159 (7)0.0032 (5)0.0080 (6)0.0085 (6)
C110.0211 (10)0.0155 (9)0.0121 (9)0.0020 (7)0.0059 (8)0.0047 (7)
C120.0202 (10)0.0231 (10)0.0269 (11)0.0036 (8)0.0095 (9)0.0133 (9)
C130.0241 (11)0.0272 (11)0.0268 (11)0.0092 (9)0.0100 (9)0.0147 (9)
C140.0355 (12)0.0181 (10)0.0184 (10)0.0079 (9)0.0123 (9)0.0095 (8)
C150.0290 (11)0.0203 (10)0.0204 (10)0.0006 (9)0.0115 (9)0.0085 (8)
C160.0209 (10)0.0210 (10)0.0157 (10)0.0038 (8)0.0071 (8)0.0081 (8)
C210.0161 (9)0.0171 (9)0.0181 (10)0.0029 (7)0.0053 (8)0.0052 (8)
C220.0271 (11)0.0188 (10)0.0254 (11)0.0049 (8)0.0124 (9)0.0098 (9)
C230.0289 (11)0.0174 (10)0.0357 (13)0.0016 (9)0.0128 (10)0.0085 (9)
C240.0221 (11)0.0193 (11)0.0275 (12)0.0018 (8)0.0016 (9)0.0001 (9)
C250.0288 (11)0.0307 (12)0.0172 (11)0.0041 (9)0.0045 (9)0.0043 (9)
C260.0252 (11)0.0248 (11)0.0190 (10)0.0021 (9)0.0068 (9)0.0088 (9)
C310.0175 (9)0.0160 (9)0.0208 (10)0.0034 (7)0.0075 (8)0.0110 (8)
C320.0240 (10)0.0234 (10)0.0201 (11)0.0059 (8)0.0097 (9)0.0108 (9)
C330.0255 (11)0.0314 (12)0.0292 (12)0.0111 (9)0.0168 (10)0.0164 (10)
C340.0167 (10)0.0384 (13)0.0348 (13)0.0077 (9)0.0075 (9)0.0213 (11)
C350.0240 (11)0.0318 (12)0.0226 (12)0.0034 (9)0.0025 (9)0.0111 (10)
C360.0240 (10)0.0212 (10)0.0202 (10)0.0054 (8)0.0083 (9)0.0094 (8)
C410.0207 (10)0.0223 (10)0.0125 (9)0.0055 (8)0.0063 (8)0.0078 (8)
C420.0310 (11)0.0236 (11)0.0205 (11)0.0076 (9)0.0109 (9)0.0095 (9)
C430.0386 (13)0.0361 (13)0.0230 (11)0.0205 (11)0.0164 (10)0.0114 (10)
C440.0291 (12)0.0513 (15)0.0275 (12)0.0114 (11)0.0187 (10)0.0152 (11)
C450.0300 (12)0.0409 (14)0.0325 (13)0.0012 (10)0.0165 (10)0.0149 (11)
C460.0277 (11)0.0259 (11)0.0210 (11)0.0034 (9)0.0112 (9)0.0076 (9)
C510.0217 (10)0.0162 (9)0.0168 (10)0.0043 (8)0.0050 (8)0.0058 (8)
C520.0247 (11)0.0293 (11)0.0200 (11)0.0017 (9)0.0056 (9)0.0126 (9)
C530.0255 (11)0.0315 (12)0.0314 (12)0.0002 (9)0.0060 (10)0.0156 (10)
C540.0261 (11)0.0208 (11)0.0260 (12)0.0024 (9)0.0010 (10)0.0065 (9)
C550.0323 (12)0.0262 (11)0.0157 (11)0.0075 (9)0.0046 (9)0.0048 (9)
C560.0280 (11)0.0222 (10)0.0186 (10)0.0049 (8)0.0092 (9)0.0072 (8)
C610.0199 (9)0.0165 (9)0.0207 (10)0.0048 (7)0.0115 (8)0.0088 (8)
C620.0312 (11)0.0253 (11)0.0186 (11)0.0092 (9)0.0109 (9)0.0095 (9)
C630.0358 (12)0.0264 (11)0.0311 (12)0.0142 (10)0.0168 (10)0.0172 (10)
C640.0345 (12)0.0180 (11)0.0381 (13)0.0101 (9)0.0220 (11)0.0098 (10)
C650.0342 (12)0.0221 (11)0.0254 (12)0.0052 (9)0.0128 (10)0.0039 (9)
C660.0266 (11)0.0207 (10)0.0220 (11)0.0048 (8)0.0089 (9)0.0081 (9)
O810.0697 (13)0.0357 (10)0.0392 (11)0.0039 (9)0.0253 (10)0.0100 (8)
C82A0.103 (3)0.069 (2)0.0462 (18)0.051 (2)0.0293 (19)0.0284 (17)
C83A0.089 (8)0.029 (3)0.057 (4)0.014 (3)0.039 (4)0.020 (3)
C84A0.0639 (19)0.0450 (17)0.0446 (17)0.0121 (14)0.0159 (15)0.0121 (14)
C850.0464 (15)0.0385 (14)0.0507 (16)0.0140 (11)0.0279 (13)0.0252 (13)
C84B0.0639 (19)0.0450 (17)0.0446 (17)0.0121 (14)0.0159 (15)0.0121 (14)
C82B0.103 (3)0.069 (2)0.0462 (18)0.051 (2)0.0293 (19)0.0284 (17)
C83B0.040 (5)0.036 (3)0.045 (4)0.016 (3)0.023 (3)0.016 (3)
O710.0862 (17)0.0474 (12)0.0529 (13)0.0363 (11)0.0367 (12)0.0199 (10)
C720.0319 (14)0.0630 (19)0.0266 (14)0.0044 (12)0.0101 (11)0.0067 (13)
C730.0393 (13)0.0253 (12)0.0308 (13)0.0002 (10)0.0108 (11)0.0087 (10)
C740.0348 (14)0.0456 (15)0.0373 (15)0.0020 (11)0.0064 (12)0.0194 (12)
C750.0512 (18)0.0339 (15)0.0561 (19)0.0043 (13)0.0144 (15)0.0247 (14)
Geometric parameters (Å, º) top
Zn—Cl12.2108 (6)C16—H1610.92 (2)
Zn—Cl22.2165 (6)C22—H2210.95 (3)
Zn—O11.9851 (15)C23—H2310.91 (3)
Zn—O21.9751 (15)C24—H2410.94 (2)
P1—O21.5039 (15)C25—H2510.96 (3)
P1—C111.794 (2)C26—H2610.88 (3)
P1—C211.789 (2)C32—H3210.95 (2)
P1—C311.791 (2)C33—H3310.90 (3)
P2—O11.5031 (15)C34—H3410.97 (3)
P2—C411.792 (2)C35—H3510.98 (3)
P2—C511.789 (2)C36—H3610.95 (3)
P2—C611.794 (2)C42—H4210.92 (3)
O81—C82A1.405 (5)C43—H4310.88 (3)
O81—C851.420 (3)C44—H4410.93 (3)
O81—C82B1.405 (5)C45—H4510.97 (3)
O71—C751.402 (5)C46—H4610.98 (3)
O71—C721.434 (4)C52—H5210.95 (3)
C11—C161.386 (3)C53—H5310.96 (3)
C11—C121.394 (3)C54—H5410.90 (3)
C12—C131.385 (3)C55—H5510.95 (3)
C13—C141.381 (3)C56—H5610.97 (3)
C14—C151.376 (3)C62—H6210.88 (3)
C15—C161.389 (3)C63—H6310.93 (3)
C21—C221.391 (3)C64—H6410.92 (3)
C21—C261.388 (3)C65—H6510.93 (3)
C22—C231.385 (3)C66—H6610.93 (3)
C23—C241.382 (3)C82A—C83A1.537 (8)
C24—C251.377 (4)C82B—C83B1.494 (9)
C25—C261.388 (3)C83A—C84A1.415 (8)
C31—C361.388 (3)C83B—C84B1.496 (9)
C31—C321.395 (3)C84A—C851.494 (5)
C32—C331.380 (3)C84B—C851.494 (5)
C33—C341.381 (3)C82A—H8210.9903
C34—C351.383 (3)C82A—H8220.9900
C35—C361.385 (3)C82B—H8230.9898
C41—C461.386 (3)C82B—H8240.9894
C41—C421.395 (3)C83A—H8320.9896
C42—C431.375 (3)C83A—H8310.9905
C43—C441.379 (4)C83B—H8340.9894
C44—C451.382 (4)C83B—H8330.9901
C45—C461.386 (4)C84A—H8420.9901
C51—C561.394 (3)C84A—H8410.9885
C51—C521.390 (3)C84B—H8440.9899
C52—C531.382 (3)C84B—H8430.9900
C53—C541.385 (3)C85—H8510.9903
C54—C551.381 (4)C85—H8520.9914
C55—C561.383 (3)C72—C731.496 (4)
C61—C621.392 (3)C73—C741.504 (4)
C61—C661.386 (3)C74—C751.491 (4)
C62—C631.384 (4)C72—H7210.94 (4)
C63—C641.377 (3)C72—H7220.97 (4)
C64—C651.381 (3)C73—H7310.99 (4)
C65—C661.390 (3)C73—H7321.05 (3)
C12—H1210.94 (3)C74—H7410.95 (3)
C13—H1310.95 (2)C74—H7420.96 (4)
C14—H1410.93 (3)C75—H7511.00 (4)
C15—H1510.92 (3)C75—H7520.98 (4)
Cl1—Zn—Cl2120.55 (2)C35—C36—H361119.7 (15)
Cl1—Zn—O1110.09 (4)C41—C42—H421119.1 (16)
Cl1—Zn—O2107.43 (4)C43—C42—H421121.0 (16)
Cl2—Zn—O1107.77 (4)C44—C43—H431121.8 (17)
Cl2—Zn—O2110.55 (4)C42—C43—H431118.0 (17)
O1—Zn—O298.16 (6)C43—C44—H441120.4 (17)
O2—P1—C11111.29 (9)C45—C44—H441119.3 (17)
O2—P1—C21111.85 (9)C44—C45—H451120 (2)
O2—P1—C31109.09 (9)C46—C45—H451120 (2)
C11—P1—C21108.60 (10)C45—C46—H461118.9 (15)
C11—P1—C31107.51 (10)C41—C46—H461121.2 (15)
C21—P1—C31108.36 (10)C51—C52—H521119.4 (16)
O1—P2—C41111.83 (9)C53—C52—H521120.5 (16)
O1—P2—C51112.21 (9)C52—C53—H531120.4 (15)
O1—P2—C61108.73 (9)C54—C53—H531119.8 (15)
C41—P2—C51108.52 (10)C53—C54—H541124.7 (16)
C41—P2—C61107.94 (11)C55—C54—H541115.1 (16)
C51—P2—C61107.43 (10)C54—C55—H551121.5 (16)
Zn—O1—P2139.20 (9)C56—C55—H551117.9 (16)
Zn—O2—P1141.01 (9)C55—C56—H561122.4 (15)
C82B—O81—C85109.4 (2)C51—C56—H561118.2 (15)
C82A—O81—C85109.4 (2)C61—C62—H621121.6 (18)
C72—O71—C75108.2 (2)C63—C62—H621118.6 (18)
C12—C11—C16119.5 (2)C62—C63—H631121.6 (17)
P1—C11—C16121.95 (17)C64—C63—H631118.0 (17)
P1—C11—C12118.43 (17)C65—C64—H641120.6 (16)
C11—C12—C13120.0 (2)C63—C64—H641119.1 (16)
C12—C13—C14120.2 (2)C64—C65—H651120.9 (17)
C13—C14—C15120.2 (2)C66—C65—H651119.1 (17)
C14—C15—C16120.2 (2)C61—C66—H661121.2 (16)
C11—C16—C15120.0 (2)C65—C66—H661118.9 (16)
P1—C21—C26121.67 (17)O81—C82A—C83A105.6 (4)
P1—C21—C22118.35 (16)O81—C82B—C83B106.7 (4)
C22—C21—C26119.9 (2)C82A—C83A—C84A104.6 (5)
C21—C22—C23119.8 (2)C82B—C83B—C84B102.9 (6)
C22—C23—C24120.0 (2)C83A—C84A—C85105.0 (4)
C23—C24—C25120.4 (2)C83B—C84B—C85105.3 (3)
C24—C25—C26120.0 (2)O81—C85—C84A107.2 (2)
C21—C26—C25119.8 (2)O81—C85—C84B107.2 (2)
P1—C31—C36118.36 (17)O81—C82A—H822110.58
C32—C31—C36119.8 (2)C83A—C82A—H821110.60
P1—C31—C32121.80 (16)O81—C82A—H821110.61
C31—C32—C33119.8 (2)H821—C82A—H822108.76
C32—C33—C34120.3 (2)C83A—C82A—H822110.70
C33—C34—C35120.2 (2)O81—C82B—H824110.33
C34—C35—C36120.1 (2)O81—C82B—H823110.38
C31—C36—C35119.9 (2)H823—C82B—H824108.70
C42—C41—C46119.8 (2)C83B—C82B—H823110.35
P2—C41—C46121.51 (17)C83B—C82B—H824110.42
P2—C41—C42118.48 (18)C82A—C83A—H831110.75
C41—C42—C43119.9 (2)C84A—C83A—H831110.84
C42—C43—C44120.2 (2)C84A—C83A—H832110.87
C43—C44—C45120.3 (2)H831—C83A—H832108.89
C44—C45—C46119.9 (2)C82A—C83A—H832110.82
C41—C46—C45119.9 (2)C82B—C83B—H833111.20
C52—C51—C56120.0 (2)C82B—C83B—H834111.16
P2—C51—C52117.87 (16)H833—C83B—H834109.16
P2—C51—C56122.11 (17)C84B—C83B—H834111.17
C51—C52—C53120.1 (2)C84B—C83B—H833111.19
C52—C53—C54119.8 (2)C83A—C84A—H841110.76
C53—C54—C55120.2 (2)C83A—C84A—H842110.78
C54—C55—C56120.5 (2)C85—C84A—H841110.74
C51—C56—C55119.4 (2)C85—C84A—H842110.70
P2—C61—C66118.62 (17)H841—C84A—H842108.88
P2—C61—C62121.53 (16)C85—C84B—H844110.71
C62—C61—C66119.8 (2)C85—C84B—H843110.64
C61—C62—C63119.8 (2)H843—C84B—H844108.83
C62—C63—C64120.3 (2)C83B—C84B—H843110.65
C63—C64—C65120.2 (2)C83B—C84B—H844110.72
C64—C65—C66120.0 (2)O81—C85—H852110.29
C61—C66—C65119.9 (2)C84A—C85—H851110.34
C11—C12—H121116.7 (17)C84A—C85—H852110.28
C13—C12—H121123.3 (17)H851—C85—H852108.52
C12—C13—H131119.1 (16)C84B—C85—H851110.34
C14—C13—H131120.7 (16)C84B—C85—H852110.28
C13—C14—H141119.9 (16)O81—C85—H851110.23
C15—C14—H141120.0 (16)O71—C72—C73105.4 (2)
C14—C15—H151119.7 (17)C72—C73—C74102.1 (2)
C16—C15—H151119.9 (17)C73—C74—C75104.1 (3)
C15—C16—H161120.0 (16)O71—C75—C74108.5 (3)
C11—C16—H161120.0 (16)O71—C72—H721108 (3)
C21—C22—H221121.2 (17)O71—C72—H722105 (2)
C23—C22—H221118.9 (17)C73—C72—H721112 (2)
C22—C23—H231119.7 (17)C73—C72—H722116 (2)
C24—C23—H231120.2 (17)H721—C72—H722109 (3)
C23—C24—H241121.7 (15)C72—C73—H731114 (2)
C25—C24—H241117.8 (15)C72—C73—H732109.7 (15)
C24—C25—H251122.1 (17)C74—C73—H731112 (2)
C26—C25—H251117.9 (17)C74—C73—H732112.4 (15)
C21—C26—H261118.7 (16)H731—C73—H732107 (3)
C25—C26—H261121.5 (16)C73—C74—H741110 (2)
C31—C32—H321120.6 (16)C73—C74—H742110 (2)
C33—C32—H321119.6 (15)C75—C74—H741113 (2)
C34—C33—H331118.9 (16)C75—C74—H742108 (2)
C32—C33—H331120.8 (16)H741—C74—H742112 (3)
C33—C34—H341117.9 (14)O71—C75—H751113 (3)
C35—C34—H341121.9 (14)O71—C75—H752109 (2)
C34—C35—H351120.2 (15)C74—C75—H751111 (3)
C36—C35—H351119.7 (15)C74—C75—H752115 (2)
C31—C36—H361120.4 (15)H751—C75—H752101 (4)

Experimental details

Crystal data
Chemical formula[ZnCl2(C18H15OP)2]·2C4H8O
Mr837.04
Crystal system, space groupTriclinic, P1
Temperature (K)123
a, b, c (Å)11.6758 (1), 12.9704 (1), 15.2874 (2)
α, β, γ (°)110.2721 (4), 109.8102 (5), 92.8572 (4)
V3)2006.16 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.87
Crystal size (mm)0.69 × 0.61 × 0.45
Data collection
DiffractometerNonius κ-CCD
diffractometer
Absorption correctionMulti-scan
applied during the scaling procedure (Nonius, 2000)
Tmin, Tmax0.559, 0.677
No. of measured, independent and
observed [I > 2σ(I)] reflections
30256, 7358, 6793
Rint0.046
(sin θ/λ)max1)0.604
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.087, 1.05
No. of reflections7357
No. of parameters640
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.54, 0.45

Computer programs: Kappa-CCD Control Software (Nonius, 2000), DENZO (Nonius, 2000), DENZO, SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1998), PLATON (Spek, 2000), PLATON.

Selected geometric parameters (Å, º) top
Zn—Cl12.2108 (6)P1—C211.789 (2)
Zn—Cl22.2165 (6)P1—C311.791 (2)
Zn—O11.9851 (15)P2—O11.5031 (15)
Zn—O21.9751 (15)P2—C411.792 (2)
P1—O21.5039 (15)P2—C511.789 (2)
P1—C111.794 (2)P2—C611.794 (2)
Cl1—Zn—Cl2120.55 (2)C41—P2—C61107.94 (11)
Cl1—Zn—O1110.09 (4)C51—P2—C61107.43 (10)
Cl1—Zn—O2107.43 (4)Zn—O1—P2139.20 (9)
Cl2—Zn—O1107.77 (4)Zn—O2—P1141.01 (9)
Cl2—Zn—O2110.55 (4)P1—C11—C16121.95 (17)
O1—Zn—O298.16 (6)P1—C11—C12118.43 (17)
O2—P1—C11111.29 (9)P1—C21—C26121.67 (17)
O2—P1—C21111.85 (9)P1—C21—C22118.35 (16)
O2—P1—C31109.09 (9)P1—C31—C36118.36 (17)
C11—P1—C21108.60 (10)P1—C31—C32121.80 (16)
C11—P1—C31107.51 (10)P2—C41—C46121.51 (17)
C21—P1—C31108.36 (10)P2—C41—C42118.48 (18)
O1—P2—C41111.83 (9)P2—C51—C52117.87 (16)
O1—P2—C51112.21 (9)P2—C51—C56122.11 (17)
O1—P2—C61108.73 (9)P2—C61—C66118.62 (17)
C41—P2—C51108.52 (10)P2—C61—C62121.53 (16)
 

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