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Acta Cryst. (2007). E63, m2359    [ doi:10.1107/S1600536807039700 ]

Bis(thiocyanato-[kappa]N)bis(triphenylphosphine oxide-[kappa]O)zinc(II)

Y. Li

Abstract top

The title compound, [Zn(NCS)2{(C6H5)3PO}2], crystallizes with two molecules in the asymmetric unit. The coordination environment of the Zn atom is distorted tetrahedral.

Comment top

Some [(C6H5)3PO]2NiX2 complexes (X = Cl, Br, I) were prepared (Cotton & Goodgame, 1960) and their electronic spectra, IR spectra and magnetic moments were recorded and analyzed in order to demonstrate that the Ni ion, in each case, was tetrahedrally coordinated. Recently, the structure of [(C6H5)3PO]2ZnCl2 had been reported (Zeller et al., 2001). Here we report the structure of [(C6H5)3PO]2Zn(SCN)2 as shown in Fig. 1.

The Zn atom is tetrahedrally coordinated. The analogous dichlorobis(triphenylphosphine oxide)zinc(II) compound (Zeller et al., 2001) has comparable geometric parameters.

Related literature top

The corresponding four-coordinate complex dichlorobis(triphenylphosphine oxide)zinc(II) has been reported by Zeller et al. (2001).

For related literature, see: Cotton & Goodgame (1960). For synthesis, see: Pinkas et al. (1998).

Experimental top

The title compound was synthesized according to a method described previously (Pinkas et al., 1998). The product of this synthesis was recrystallized by slow evaporation of an acetone solution at room temperature to give yellow block shaped crystals. Analysis calculated for C38H30N2O2P2S2Zn: C 61.83, H 4.10, N 3.80%; foud (%): C 61.48, H 4.49, N 3.67%.

Refinement top

All H atoms were placed at geometrically idealized positions and were treated as riding, with C—H = 0.93Å and Uiso(H) = 1.2Ueq(partent atom).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2000).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level.
Bis(thiocyanato-κN)bis(triphenylphosphine oxide-κO)zinc(II) top
Crystal data top
[Zn1(N1C1S1)2(C18H15O1P1)2]Z = 4
Mr = 738.07F000 = 1520
Triclinic, P1Dx = 1.358 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 9.9695 (6) ÅCell parameters from 22725 reflections
b = 19.6036 (12) Åθ = 2.2–28.2º
c = 21.2407 (12) ŵ = 0.92 mm−1
α = 116.799 (3)ºT = 298 (2) K
β = 98.316 (3)ºBlock, yellow
γ = 95.098 (3)º0.20 × 0.15 × 0.12 mm
V = 3610.2 (4) Å3
Data collection top
Siemens SMART CCD
diffractometer		12513 independent reflections
Radiation source: fine-focus sealed tube10612 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.057
T = 298(2) Kθmax = 25.0º
ω scansθmin = 1.1º
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)		h = −11→11
Tmin = 0.837, Tmax = 0.898k = −23→16
37146 measured reflectionsl = −23→25
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.091  w = 1/[σ2(Fo2) + (0.0405P)2 + 0.9616P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
12513 reflectionsΔρmax = 0.45 e Å−3
847 parametersΔρmin = −0.48 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Zn1(N1C1S1)2(C18H15O1P1)2]γ = 95.098 (3)º
Mr = 738.07V = 3610.2 (4) Å3
Triclinic, P1Z = 4
a = 9.9695 (6) ÅMo Kα
b = 19.6036 (12) ŵ = 0.92 mm−1
c = 21.2407 (12) ÅT = 298 (2) K
α = 116.799 (3)º0.20 × 0.15 × 0.12 mm
β = 98.316 (3)º
Data collection top
Siemens SMART CCD
diffractometer		12513 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)		10612 reflections with I > 2σ(I)
Tmin = 0.837, Tmax = 0.898Rint = 0.057
37146 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032847 parameters
wR(F2) = 0.091H-atom parameters constrained
S = 1.07Δρmax = 0.45 e Å−3
12513 reflectionsΔρmin = −0.48 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
xyzUiso*/Ueq
Zn10.13192 (2)1.052920 (13)0.847081 (13)0.04077 (7)
Zn20.56423 (2)0.630566 (14)0.368980 (13)0.04653 (8)
S1−0.08062 (8)1.26379 (4)0.88646 (4)0.0737 (2)
S20.45853 (9)1.23027 (5)1.04395 (5)0.0906 (3)
S30.53990 (8)0.89535 (4)0.48324 (4)0.0757 (2)
S40.75445 (13)0.51796 (5)0.50542 (5)0.1086 (4)
P10.25043 (5)0.96611 (3)0.69865 (3)0.04347 (13)
P2−0.10195 (5)0.91425 (3)0.83896 (3)0.04148 (13)
P30.74093 (5)0.62405 (3)0.24295 (3)0.04247 (13)
P40.31137 (5)0.49654 (3)0.26626 (3)0.04336 (13)
O10.21036 (16)0.98176 (9)0.76912 (8)0.0544 (4)
O2−0.00785 (17)0.98849 (9)0.86071 (9)0.0616 (4)
O30.65577 (16)0.60806 (10)0.28875 (9)0.0599 (4)
O40.37749 (14)0.57989 (8)0.31675 (9)0.0551 (4)
N10.0359 (2)1.13118 (12)0.83707 (12)0.0614 (5)
N20.2797 (2)1.10586 (12)0.93108 (11)0.0611 (5)
N30.5642 (2)0.74096 (13)0.41903 (12)0.0692 (6)
N40.6444 (3)0.58588 (14)0.42612 (13)0.0782 (7)
C1−0.0123 (2)1.18685 (14)0.85828 (12)0.0490 (5)
C20.3557 (2)1.15767 (13)0.97794 (12)0.0495 (5)
C30.1311 (2)0.99525 (13)0.64781 (12)0.0489 (5)
C40.1331 (3)1.07421 (16)0.67189 (17)0.0763 (8)
H40.20231.11030.70990.092*
C50.0335 (4)1.0991 (2)0.6398 (2)0.0942 (10)
H50.03611.15200.65610.113*
C6−0.0686 (3)1.0476 (2)0.5848 (2)0.0893 (10)
H6−0.13671.06530.56420.107*
C7−0.0719 (3)0.9698 (2)0.55953 (19)0.0881 (10)
H7−0.14140.93450.52120.106*
C80.0285 (2)0.94324 (17)0.59094 (15)0.0673 (7)
H80.02640.89020.57350.081*
C90.4192 (2)1.01616 (12)0.71102 (11)0.0460 (5)
C100.5157 (2)1.03588 (13)0.77341 (13)0.0532 (5)
H100.49001.02770.81020.064*
C110.6501 (2)1.06763 (14)0.78059 (15)0.0617 (6)
H110.71431.08120.82250.074*
C120.6893 (2)1.07927 (15)0.72641 (15)0.0632 (7)
H120.78041.09960.73120.076*
C130.5940 (3)1.06093 (16)0.66515 (14)0.0666 (7)
H130.62041.06960.62870.080*
C140.4593 (2)1.02972 (15)0.65734 (13)0.0588 (6)
H140.39511.01770.61580.071*
C150.2511 (2)0.86410 (12)0.64717 (12)0.0454 (5)
C160.3470 (2)0.83581 (14)0.60491 (14)0.0632 (7)
H160.41410.87030.60280.076*
C170.3439 (3)0.75717 (16)0.56604 (16)0.0752 (8)
H170.40900.73910.53800.090*
C180.2457 (3)0.70546 (15)0.56835 (16)0.0699 (7)
H180.24400.65240.54210.084*
C190.1498 (3)0.73258 (15)0.60967 (17)0.0749 (8)
H190.08220.69760.61100.090*
C200.1525 (3)0.81102 (14)0.64913 (15)0.0640 (7)
H200.08750.82860.67740.077*
C21−0.1479 (2)0.85453 (12)0.74305 (11)0.0441 (5)
C22−0.1879 (2)0.88990 (16)0.70127 (14)0.0608 (6)
H22−0.18180.94350.72270.073*
C23−0.2365 (3)0.8456 (2)0.62824 (16)0.0796 (9)
H23−0.26480.86920.60040.096*
C24−0.2433 (3)0.7667 (2)0.59641 (16)0.0851 (10)
H24−0.27560.73710.54690.102*
C25−0.2033 (3)0.73135 (17)0.63665 (15)0.0759 (8)
H25−0.20760.67780.61440.091*
C26−0.1563 (2)0.77469 (13)0.71037 (13)0.0559 (6)
H26−0.13030.75040.73790.067*
C27−0.0242 (2)0.85997 (12)0.87847 (11)0.0457 (5)
C280.1077 (2)0.84514 (16)0.86907 (14)0.0638 (7)
H280.15080.86080.84050.077*
C290.1739 (3)0.80750 (18)0.90191 (17)0.0814 (9)
H290.26180.79760.89550.098*
C300.1110 (4)0.78457 (17)0.94402 (17)0.0841 (9)
H300.15670.75950.96650.101*
C31−0.0192 (4)0.79833 (18)0.95330 (17)0.0808 (8)
H31−0.06140.78240.98190.097*
C32−0.0876 (3)0.83564 (15)0.92060 (14)0.0635 (6)
H32−0.17610.84450.92670.076*
C33−0.2620 (2)0.93378 (12)0.86656 (12)0.0441 (5)
C34−0.3809 (2)0.87841 (14)0.83064 (15)0.0653 (7)
H34−0.37740.83020.79320.078*
C35−0.5050 (3)0.89542 (16)0.85093 (17)0.0702 (7)
H35−0.58450.85810.82740.084*
C36−0.5110 (3)0.96633 (17)0.90499 (14)0.0627 (7)
H36−0.59470.97750.91800.075*
C37−0.3951 (3)1.02105 (16)0.94019 (14)0.0663 (7)
H37−0.40031.06940.97700.080*
C38−0.2685 (2)1.00533 (14)0.92164 (12)0.0552 (6)
H38−0.18941.04270.94620.066*
C390.5547 (2)0.80563 (14)0.44501 (12)0.0509 (5)
C400.6879 (3)0.55690 (16)0.45897 (14)0.0682 (7)
C410.6649 (2)0.68279 (12)0.20796 (12)0.0454 (5)
C420.5521 (3)0.71419 (17)0.23084 (16)0.0727 (8)
H420.51980.70850.26750.087*
C430.4862 (3)0.7542 (2)0.19961 (19)0.0940 (10)
H430.40940.77480.21510.113*
C440.5331 (3)0.76350 (16)0.14668 (16)0.0737 (8)
H440.48730.78950.12530.088*
C450.6471 (3)0.73484 (18)0.12472 (18)0.0776 (8)
H450.68070.74250.08940.093*
C460.7125 (3)0.69439 (18)0.15505 (17)0.0735 (8)
H460.78990.67460.13960.088*
C470.9126 (2)0.67214 (13)0.29397 (13)0.0491 (5)
C480.9381 (3)0.69812 (17)0.36752 (15)0.0719 (7)
H480.86880.68830.38890.086*
C491.0668 (3)0.7388 (2)0.40967 (19)0.0947 (10)
H491.08340.75650.45920.114*
C501.1686 (3)0.75293 (18)0.3787 (2)0.0931 (11)
H501.25490.77990.40710.112*
C511.1447 (3)0.72767 (18)0.3063 (2)0.0865 (10)
H511.21500.73760.28560.104*
C521.0162 (2)0.68712 (15)0.26282 (16)0.0686 (7)
H521.00030.67030.21340.082*
C530.7476 (2)0.53510 (12)0.16532 (12)0.0432 (5)
C540.8561 (3)0.49588 (15)0.16201 (16)0.0683 (7)
H540.93300.51710.19960.082*
C550.8510 (3)0.42478 (16)0.10277 (19)0.0873 (10)
H550.92550.39890.10030.105*
C560.7372 (3)0.39215 (15)0.04772 (16)0.0739 (8)
H560.73430.34430.00810.089*
C570.6274 (3)0.43035 (16)0.05126 (15)0.0728 (7)
H570.54920.40790.01440.087*
C580.6327 (2)0.50157 (15)0.10901 (14)0.0619 (6)
H580.55880.52770.11060.074*
C590.2675 (2)0.48219 (14)0.17566 (13)0.0502 (5)
C600.2558 (3)0.54711 (18)0.16597 (17)0.0772 (8)
H600.27440.59630.20570.093*
C610.2165 (4)0.5387 (2)0.0977 (2)0.1054 (12)
H610.20750.58230.09150.126*
C620.1910 (4)0.4678 (3)0.0395 (2)0.0995 (11)
H620.16530.4630−0.00640.119*
C630.2026 (3)0.4026 (2)0.04727 (16)0.0835 (9)
H630.18450.35390.00690.100*
C640.2415 (3)0.40969 (16)0.11559 (14)0.0647 (7)
H640.25010.36570.12110.078*
C650.4176 (2)0.42756 (12)0.26716 (12)0.0455 (5)
C660.5101 (2)0.40487 (15)0.22166 (14)0.0626 (6)
H660.51430.42340.18850.075*
C670.5954 (3)0.35495 (18)0.22573 (16)0.0778 (9)
H670.65700.33930.19510.093*
C680.5896 (3)0.32809 (15)0.27513 (18)0.0768 (9)
H680.64570.29330.27690.092*
C690.5016 (3)0.35221 (18)0.32184 (19)0.0788 (9)
H690.50050.33530.35630.095*
C700.4145 (2)0.40171 (16)0.31761 (16)0.0646 (7)
H700.35370.41760.34880.077*
C710.15697 (19)0.47608 (12)0.29288 (12)0.0435 (5)
C720.0756 (2)0.40260 (14)0.25765 (14)0.0582 (6)
H720.09880.36300.21800.070*
C73−0.0393 (2)0.38894 (16)0.28186 (16)0.0701 (7)
H73−0.09330.33970.25870.084*
C74−0.0753 (2)0.44714 (17)0.33991 (16)0.0696 (7)
H74−0.15310.43730.35590.084*
C750.0033 (3)0.51953 (16)0.37412 (15)0.0697 (7)
H75−0.02170.55900.41320.084*
C760.1194 (2)0.53448 (14)0.35106 (13)0.0584 (6)
H760.17250.58390.37460.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.03915 (12)0.03626 (13)0.04320 (14)0.00350 (9)0.00903 (10)0.01595 (11)
Zn20.04996 (14)0.04471 (15)0.04040 (14)0.00410 (11)0.00907 (10)0.01699 (12)
S10.0772 (4)0.0592 (4)0.0834 (5)0.0265 (3)0.0200 (4)0.0290 (4)
S20.0891 (5)0.0618 (4)0.0803 (5)−0.0048 (4)−0.0310 (4)0.0161 (4)
S30.0885 (5)0.0505 (4)0.0766 (5)0.0154 (3)0.0079 (4)0.0225 (4)
S40.1950 (11)0.0843 (6)0.0607 (5)0.0675 (6)0.0265 (6)0.0385 (4)
P10.0471 (3)0.0440 (3)0.0416 (3)0.0107 (2)0.0150 (2)0.0198 (3)
P20.0433 (3)0.0378 (3)0.0433 (3)0.0040 (2)0.0161 (2)0.0175 (2)
P30.0393 (3)0.0442 (3)0.0480 (3)0.0103 (2)0.0128 (2)0.0237 (3)
P40.0381 (3)0.0402 (3)0.0513 (3)0.0066 (2)0.0111 (2)0.0206 (3)
O10.0659 (9)0.0591 (9)0.0481 (9)0.0216 (8)0.0273 (7)0.0272 (8)
O20.0674 (10)0.0462 (9)0.0632 (10)−0.0080 (7)0.0266 (8)0.0184 (8)
O30.0622 (9)0.0656 (10)0.0632 (10)0.0136 (8)0.0291 (8)0.0350 (9)
O40.0464 (8)0.0405 (8)0.0686 (11)0.0032 (6)0.0113 (7)0.0183 (8)
N10.0599 (12)0.0569 (13)0.0732 (14)0.0161 (10)0.0121 (10)0.0349 (11)
N20.0515 (11)0.0559 (12)0.0576 (13)0.0042 (9)−0.0009 (9)0.0155 (11)
N30.0771 (14)0.0505 (13)0.0616 (14)0.0067 (11)0.0115 (11)0.0123 (11)
N40.1013 (18)0.0761 (16)0.0599 (14)0.0168 (13)0.0049 (12)0.0375 (13)
C10.0462 (11)0.0522 (14)0.0499 (13)0.0048 (10)0.0054 (9)0.0272 (11)
C20.0481 (12)0.0517 (13)0.0497 (13)0.0144 (10)0.0058 (10)0.0250 (12)
C30.0500 (12)0.0564 (14)0.0470 (13)0.0125 (10)0.0166 (10)0.0277 (11)
C40.093 (2)0.0579 (16)0.0744 (19)0.0222 (14)0.0061 (15)0.0295 (15)
C50.119 (3)0.085 (2)0.098 (3)0.050 (2)0.025 (2)0.054 (2)
C60.0753 (19)0.126 (3)0.108 (3)0.041 (2)0.0258 (19)0.084 (3)
C70.0593 (16)0.121 (3)0.092 (2)−0.0030 (17)−0.0059 (15)0.067 (2)
C80.0576 (14)0.0720 (17)0.0752 (18)0.0029 (12)0.0040 (13)0.0415 (15)
C90.0497 (11)0.0436 (12)0.0422 (12)0.0079 (9)0.0107 (9)0.0177 (10)
C100.0613 (13)0.0512 (13)0.0517 (14)0.0093 (11)0.0074 (10)0.0294 (11)
C110.0562 (13)0.0604 (15)0.0651 (16)0.0057 (11)−0.0060 (11)0.0328 (13)
C120.0491 (13)0.0596 (15)0.0751 (18)0.0017 (11)0.0074 (12)0.0298 (14)
C130.0651 (15)0.0759 (18)0.0568 (15)−0.0043 (13)0.0156 (12)0.0317 (14)
C140.0559 (13)0.0706 (16)0.0431 (13)−0.0036 (11)0.0051 (10)0.0249 (12)
C150.0461 (11)0.0447 (12)0.0470 (12)0.0109 (9)0.0134 (9)0.0215 (10)
C160.0613 (14)0.0537 (15)0.0708 (17)0.0101 (12)0.0286 (13)0.0219 (13)
C170.0787 (18)0.0626 (17)0.0791 (19)0.0256 (14)0.0353 (15)0.0212 (15)
C180.0850 (18)0.0477 (14)0.0730 (18)0.0210 (13)0.0141 (14)0.0239 (13)
C190.0836 (18)0.0506 (15)0.099 (2)0.0116 (13)0.0307 (16)0.0390 (16)
C200.0694 (15)0.0546 (15)0.0822 (18)0.0164 (12)0.0359 (13)0.0374 (14)
C210.0405 (10)0.0466 (12)0.0464 (12)0.0056 (9)0.0152 (9)0.0216 (10)
C220.0639 (14)0.0674 (16)0.0608 (16)0.0182 (12)0.0163 (12)0.0363 (14)
C230.0683 (17)0.119 (3)0.0653 (19)0.0128 (17)0.0055 (14)0.058 (2)
C240.0741 (18)0.110 (3)0.0479 (16)−0.0131 (17)0.0020 (13)0.0252 (18)
C250.0833 (18)0.0594 (16)0.0557 (17)−0.0147 (14)0.0171 (14)0.0061 (14)
C260.0641 (14)0.0476 (13)0.0499 (14)−0.0003 (11)0.0159 (11)0.0183 (11)
C270.0459 (11)0.0450 (12)0.0401 (11)0.0056 (9)0.0074 (9)0.0156 (10)
C280.0525 (13)0.0711 (17)0.0632 (16)0.0162 (12)0.0123 (11)0.0267 (14)
C290.0705 (17)0.079 (2)0.077 (2)0.0308 (15)0.0024 (15)0.0216 (17)
C300.109 (2)0.0595 (17)0.071 (2)0.0254 (17)−0.0117 (17)0.0260 (15)
C310.105 (2)0.0759 (19)0.074 (2)0.0131 (17)0.0124 (16)0.0486 (17)
C320.0694 (15)0.0672 (16)0.0666 (17)0.0150 (13)0.0196 (13)0.0403 (14)
C330.0491 (11)0.0446 (12)0.0480 (12)0.0134 (9)0.0204 (9)0.0259 (10)
C340.0571 (14)0.0488 (14)0.0828 (18)0.0070 (11)0.0305 (13)0.0205 (13)
C350.0520 (13)0.0699 (17)0.093 (2)0.0097 (12)0.0308 (13)0.0371 (16)
C360.0594 (14)0.0856 (19)0.0661 (16)0.0326 (14)0.0321 (13)0.0462 (15)
C370.0808 (18)0.0714 (17)0.0512 (15)0.0370 (15)0.0280 (13)0.0243 (13)
C380.0621 (13)0.0567 (14)0.0431 (13)0.0164 (11)0.0125 (10)0.0187 (11)
C390.0501 (12)0.0543 (15)0.0390 (12)0.0027 (10)0.0028 (9)0.0171 (11)
C400.096 (2)0.0609 (16)0.0435 (14)0.0212 (14)0.0151 (13)0.0196 (13)
C410.0416 (10)0.0417 (11)0.0508 (13)0.0068 (9)0.0069 (9)0.0208 (10)
C420.0778 (17)0.089 (2)0.0745 (18)0.0469 (15)0.0340 (14)0.0474 (17)
C430.097 (2)0.113 (3)0.100 (3)0.071 (2)0.0377 (19)0.060 (2)
C440.0880 (19)0.0561 (16)0.0742 (19)0.0235 (14)−0.0021 (15)0.0317 (14)
C450.0848 (19)0.083 (2)0.095 (2)0.0217 (16)0.0236 (16)0.0648 (19)
C460.0600 (15)0.094 (2)0.104 (2)0.0303 (14)0.0314 (14)0.0713 (19)
C470.0438 (11)0.0442 (12)0.0569 (14)0.0115 (9)0.0054 (10)0.0225 (11)
C480.0633 (15)0.0818 (19)0.0647 (18)0.0117 (14)−0.0010 (13)0.0338 (16)
C490.078 (2)0.100 (3)0.077 (2)0.0189 (18)−0.0169 (17)0.0258 (19)
C500.0553 (17)0.0660 (19)0.118 (3)0.0117 (14)−0.0196 (18)0.020 (2)
C510.0489 (14)0.0704 (19)0.122 (3)0.0043 (13)0.0158 (16)0.031 (2)
C520.0488 (13)0.0664 (16)0.0800 (19)0.0044 (12)0.0148 (12)0.0261 (15)
C530.0430 (10)0.0407 (11)0.0502 (12)0.0076 (9)0.0137 (9)0.0240 (10)
C540.0527 (13)0.0528 (14)0.0847 (19)0.0175 (11)0.0038 (12)0.0214 (14)
C550.0745 (18)0.0554 (16)0.112 (3)0.0314 (14)0.0181 (17)0.0197 (17)
C560.093 (2)0.0468 (14)0.0705 (18)0.0160 (14)0.0227 (15)0.0154 (13)
C570.0779 (17)0.0609 (16)0.0580 (16)0.0058 (14)0.0012 (13)0.0146 (14)
C580.0554 (13)0.0632 (16)0.0614 (16)0.0173 (12)0.0089 (11)0.0243 (13)
C590.0450 (11)0.0573 (14)0.0575 (14)0.0143 (10)0.0170 (10)0.0320 (12)
C600.107 (2)0.0699 (18)0.080 (2)0.0374 (16)0.0399 (17)0.0475 (16)
C610.158 (4)0.112 (3)0.099 (3)0.065 (3)0.055 (3)0.079 (3)
C620.115 (3)0.142 (3)0.077 (2)0.049 (2)0.0295 (19)0.074 (3)
C630.087 (2)0.100 (2)0.0570 (18)0.0140 (17)0.0092 (14)0.0334 (17)
C640.0663 (15)0.0667 (17)0.0602 (16)0.0082 (12)0.0073 (12)0.0315 (14)
C650.0373 (10)0.0402 (11)0.0520 (13)0.0034 (8)0.0054 (9)0.0175 (10)
C660.0537 (13)0.0730 (17)0.0541 (15)0.0207 (12)0.0099 (11)0.0226 (13)
C670.0581 (15)0.086 (2)0.0677 (18)0.0342 (14)0.0072 (13)0.0158 (16)
C680.0541 (15)0.0528 (15)0.104 (2)0.0150 (12)−0.0092 (15)0.0267 (16)
C690.0578 (15)0.084 (2)0.121 (3)0.0120 (14)0.0068 (16)0.074 (2)
C700.0509 (13)0.0769 (18)0.0868 (19)0.0169 (12)0.0212 (12)0.0533 (16)
C710.0379 (10)0.0458 (12)0.0489 (12)0.0094 (9)0.0093 (9)0.0236 (10)
C720.0481 (12)0.0481 (13)0.0688 (16)0.0060 (10)0.0183 (11)0.0181 (12)
C730.0513 (13)0.0574 (15)0.093 (2)−0.0023 (11)0.0189 (13)0.0294 (15)
C740.0483 (13)0.0816 (19)0.0813 (19)0.0057 (13)0.0248 (13)0.0382 (17)
C750.0633 (15)0.0737 (18)0.0640 (16)0.0120 (13)0.0295 (13)0.0206 (14)
C760.0526 (13)0.0536 (14)0.0569 (15)0.0033 (11)0.0135 (11)0.0162 (12)
Geometric parameters (Å, °) top
Zn1—N21.931 (2)C30—C311.373 (5)
Zn1—O21.9376 (15)C30—H300.9300
Zn1—O11.9454 (15)C31—C321.375 (4)
Zn1—N11.952 (2)C31—H310.9300
Zn2—N41.919 (2)C32—H320.9300
Zn2—N31.934 (2)C33—C381.378 (3)
Zn2—O41.9400 (14)C33—C341.388 (3)
Zn2—O31.9429 (15)C34—C351.388 (3)
S1—C11.607 (3)C34—H340.9300
S2—C21.603 (2)C35—C361.360 (4)
S3—C391.602 (3)C35—H350.9300
S4—C401.605 (3)C36—C371.360 (4)
P1—O11.5084 (15)C36—H360.9300
P1—C91.792 (2)C37—C381.395 (3)
P1—C31.792 (2)C37—H370.9300
P1—C151.797 (2)C38—H380.9300
P2—O21.4959 (15)C41—C421.375 (3)
P2—C271.789 (2)C41—C461.380 (3)
P2—C331.793 (2)C42—C431.386 (4)
P2—C211.793 (2)C42—H420.9300
P3—O31.4939 (16)C43—C441.355 (4)
P3—C411.793 (2)C43—H430.9300
P3—C531.795 (2)C44—C451.362 (4)
P3—C471.802 (2)C44—H440.9300
P4—O41.5095 (15)C45—C461.378 (4)
P4—C711.788 (2)C45—H450.9300
P4—C591.795 (2)C46—H460.9300
P4—C651.795 (2)C47—C481.382 (4)
N1—C11.157 (3)C47—C521.382 (3)
N2—C21.153 (3)C48—C491.388 (4)
N3—C391.152 (3)C48—H480.9300
N4—C401.145 (3)C49—C501.359 (5)
C3—C81.375 (3)C49—H490.9300
C3—C41.391 (3)C50—C511.362 (5)
C4—C51.370 (4)C50—H500.9300
C4—H40.9300C51—C521.393 (4)
C5—C61.352 (5)C51—H510.9300
C5—H50.9300C52—H520.9300
C6—C71.366 (5)C53—C541.374 (3)
C6—H60.9300C53—C581.391 (3)
C7—C81.389 (4)C54—C551.384 (4)
C7—H70.9300C54—H540.9300
C8—H80.9300C55—C561.370 (4)
C9—C141.384 (3)C55—H550.9300
C9—C101.391 (3)C56—C571.372 (4)
C10—C111.383 (3)C56—H560.9300
C10—H100.9300C57—C581.371 (4)
C11—C121.372 (4)C57—H570.9300
C11—H110.9300C58—H580.9300
C12—C131.373 (4)C59—C641.385 (3)
C12—H120.9300C59—C601.390 (3)
C13—C141.380 (3)C60—C611.377 (5)
C13—H130.9300C60—H600.9300
C14—H140.9300C61—C621.350 (5)
C15—C161.385 (3)C61—H610.9300
C15—C201.386 (3)C62—C631.372 (5)
C16—C171.377 (3)C62—H620.9300
C16—H160.9300C63—C641.386 (4)
C17—C181.367 (4)C63—H630.9300
C17—H170.9300C64—H640.9300
C18—C191.371 (4)C65—C701.379 (3)
C18—H180.9300C65—C661.387 (3)
C19—C201.375 (4)C66—C671.375 (4)
C19—H190.9300C66—H660.9300
C20—H200.9300C67—C681.376 (4)
C21—C261.385 (3)C67—H670.9300
C21—C221.389 (3)C68—C691.371 (4)
C22—C231.374 (4)C68—H680.9300
C22—H220.9300C69—C701.382 (4)
C23—C241.371 (4)C69—H690.9300
C23—H230.9300C70—H700.9300
C24—C251.362 (4)C71—C761.383 (3)
C24—H240.9300C71—C721.392 (3)
C25—C261.382 (4)C72—C731.374 (3)
C25—H250.9300C72—H720.9300
C26—H260.9300C73—C741.372 (4)
C27—C321.387 (3)C73—H730.9300
C27—C281.394 (3)C74—C751.365 (4)
C28—C291.373 (4)C74—H740.9300
C28—H280.9300C75—C761.378 (3)
C29—C301.368 (5)C75—H750.9300
C29—H290.9300C76—H760.9300
N2—Zn1—O2111.57 (9)C32—C31—H31119.8
N2—Zn1—O1106.88 (8)C31—C32—C27119.8 (3)
O2—Zn1—O1105.69 (7)C31—C32—H32120.1
N2—Zn1—N1107.80 (9)C27—C32—H32120.1
O2—Zn1—N1103.88 (8)C38—C33—C34119.7 (2)
O1—Zn1—N1120.98 (8)C38—C33—P2119.87 (17)
N4—Zn2—N3116.34 (10)C34—C33—P2120.35 (17)
N4—Zn2—O4113.40 (9)C35—C34—C33119.7 (2)
N3—Zn2—O4107.47 (8)C35—C34—H34120.2
N4—Zn2—O3109.50 (9)C33—C34—H34120.2
N3—Zn2—O3108.76 (9)C36—C35—C34120.3 (2)
O4—Zn2—O3100.07 (7)C36—C35—H35119.8
O1—P1—C9112.56 (10)C34—C35—H35119.8
O1—P1—C3110.67 (9)C35—C36—C37120.3 (2)
C9—P1—C3107.94 (10)C35—C36—H36119.8
O1—P1—C15109.13 (10)C37—C36—H36119.8
C9—P1—C15107.21 (10)C36—C37—C38120.6 (2)
C3—P1—C15109.24 (11)C36—C37—H37119.7
O2—P2—C27110.57 (10)C38—C37—H37119.7
O2—P2—C33110.33 (10)C33—C38—C37119.3 (2)
C27—P2—C33109.39 (10)C33—C38—H38120.4
O2—P2—C21112.59 (10)C37—C38—H38120.4
C27—P2—C21108.77 (10)N3—C39—S3178.2 (2)
C33—P2—C21105.01 (10)N4—C40—S4177.9 (3)
O3—P3—C41111.22 (10)C42—C41—C46118.2 (2)
O3—P3—C53110.14 (10)C42—C41—P3120.25 (19)
C41—P3—C53105.46 (10)C46—C41—P3121.46 (17)
O3—P3—C47110.51 (11)C41—C42—C43120.4 (3)
C41—P3—C47109.37 (10)C41—C42—H42119.8
C53—P3—C47110.01 (10)C43—C42—H42119.8
O4—P4—C71108.46 (9)C44—C43—C42120.4 (3)
O4—P4—C59110.00 (10)C44—C43—H43119.8
C71—P4—C59108.65 (10)C42—C43—H43119.8
O4—P4—C65113.75 (9)C43—C44—C45120.2 (3)
C71—P4—C65107.38 (10)C43—C44—H44119.9
C59—P4—C65108.46 (11)C45—C44—H44119.9
P1—O1—Zn1144.35 (10)C44—C45—C46119.8 (3)
P2—O2—Zn1153.74 (11)C44—C45—H45120.1
P3—O3—Zn2157.78 (11)C46—C45—H45120.1
P4—O4—Zn2133.60 (9)C45—C46—C41121.0 (2)
C1—N1—Zn1154.5 (2)C45—C46—H46119.5
C2—N2—Zn1157.2 (2)C41—C46—H46119.5
C39—N3—Zn2174.6 (2)C48—C47—C52119.4 (2)
C40—N4—Zn2177.3 (3)C48—C47—P3118.05 (19)
N1—C1—S1179.1 (2)C52—C47—P3122.4 (2)
N2—C2—S2178.8 (2)C47—C48—C49120.2 (3)
C8—C3—C4118.6 (2)C47—C48—H48119.9
C8—C3—P1122.65 (19)C49—C48—H48119.9
C4—C3—P1118.35 (19)C50—C49—C48120.1 (3)
C5—C4—C3120.3 (3)C50—C49—H49119.9
C5—C4—H4119.9C48—C49—H49119.9
C3—C4—H4119.9C49—C50—C51120.2 (3)
C6—C5—C4120.8 (3)C49—C50—H50119.9
C6—C5—H5119.6C51—C50—H50119.9
C4—C5—H5119.6C50—C51—C52120.8 (3)
C5—C6—C7120.1 (3)C50—C51—H51119.6
C5—C6—H6119.9C52—C51—H51119.6
C7—C6—H6119.9C47—C52—C51119.2 (3)
C6—C7—C8120.1 (3)C47—C52—H52120.4
C6—C7—H7120.0C51—C52—H52120.4
C8—C7—H7120.0C54—C53—C58118.9 (2)
C3—C8—C7120.1 (3)C54—C53—P3122.70 (18)
C3—C8—H8119.9C58—C53—P3118.14 (16)
C7—C8—H8119.9C53—C54—C55120.0 (2)
C14—C9—C10119.2 (2)C53—C54—H54120.0
C14—C9—P1121.45 (17)C55—C54—H54120.0
C10—C9—P1119.15 (17)C56—C55—C54120.6 (2)
C11—C10—C9119.8 (2)C56—C55—H55119.7
C11—C10—H10120.1C54—C55—H55119.7
C9—C10—H10120.1C55—C56—C57119.7 (3)
C12—C11—C10120.5 (2)C55—C56—H56120.1
C12—C11—H11119.7C57—C56—H56120.1
C10—C11—H11119.7C58—C57—C56120.1 (3)
C11—C12—C13119.9 (2)C58—C57—H57119.9
C11—C12—H12120.1C56—C57—H57119.9
C13—C12—H12120.1C57—C58—C53120.6 (2)
C12—C13—C14120.3 (2)C57—C58—H58119.7
C12—C13—H13119.8C53—C58—H58119.7
C14—C13—H13119.8C64—C59—C60118.9 (2)
C13—C14—C9120.3 (2)C64—C59—P4123.14 (18)
C13—C14—H14119.9C60—C59—P4117.9 (2)
C9—C14—H14119.9C61—C60—C59120.1 (3)
C16—C15—C20118.1 (2)C61—C60—H60120.0
C16—C15—P1122.48 (17)C59—C60—H60120.0
C20—C15—P1119.43 (17)C62—C61—C60120.5 (3)
C17—C16—C15120.8 (2)C62—C61—H61119.8
C17—C16—H16119.6C60—C61—H61119.8
C15—C16—H16119.6C61—C62—C63120.8 (3)
C18—C17—C16120.5 (2)C61—C62—H62119.6
C18—C17—H17119.7C63—C62—H62119.6
C16—C17—H17119.7C62—C63—C64119.7 (3)
C17—C18—C19119.4 (3)C62—C63—H63120.2
C17—C18—H18120.3C64—C63—H63120.2
C19—C18—H18120.3C59—C64—C63120.0 (3)
C18—C19—C20120.6 (3)C59—C64—H64120.0
C18—C19—H19119.7C63—C64—H64120.0
C20—C19—H19119.7C70—C65—C66119.8 (2)
C19—C20—C15120.7 (2)C70—C65—P4119.25 (18)
C19—C20—H20119.7C66—C65—P4120.71 (19)
C15—C20—H20119.7C67—C66—C65119.8 (3)
C26—C21—C22119.5 (2)C67—C66—H66120.1
C26—C21—P2122.59 (18)C65—C66—H66120.1
C22—C21—P2117.70 (17)C66—C67—C68120.0 (3)
C23—C22—C21120.0 (3)C66—C67—H67120.0
C23—C22—H22120.0C68—C67—H67120.0
C21—C22—H22120.0C69—C68—C67120.5 (3)
C24—C23—C22120.0 (3)C69—C68—H68119.7
C24—C23—H23120.0C67—C68—H68119.7
C22—C23—H23120.0C68—C69—C70119.8 (3)
C25—C24—C23120.6 (3)C68—C69—H69120.1
C25—C24—H24119.7C70—C69—H69120.1
C23—C24—H24119.7C65—C70—C69120.0 (3)
C24—C25—C26120.3 (3)C65—C70—H70120.0
C24—C25—H25119.9C69—C70—H70120.0
C26—C25—H25119.9C76—C71—C72119.3 (2)
C25—C26—C21119.7 (3)C76—C71—P4118.95 (16)
C25—C26—H26120.2C72—C71—P4121.74 (17)
C21—C26—H26120.2C73—C72—C71119.6 (2)
C32—C27—C28119.3 (2)C73—C72—H72120.2
C32—C27—P2122.37 (17)C71—C72—H72120.2
C28—C27—P2118.28 (18)C74—C73—C72120.7 (2)
C29—C28—C27120.0 (3)C74—C73—H73119.7
C29—C28—H28120.0C72—C73—H73119.7
C27—C28—H28120.0C75—C74—C73120.0 (2)
C30—C29—C28120.2 (3)C75—C74—H74120.0
C30—C29—H29119.9C73—C74—H74120.0
C28—C29—H29119.9C74—C75—C76120.4 (2)
C29—C30—C31120.4 (3)C74—C75—H75119.8
C29—C30—H30119.8C76—C75—H75119.8
C31—C30—H30119.8C75—C76—C71120.1 (2)
C30—C31—C32120.4 (3)C75—C76—H76120.0
C30—C31—H31119.8C71—C76—H76120.0
Acknowledgements top

We gratefully acknowledge the support of Jingchu University of Technology and the data collection of Wuhan University.

references
References top

Cotton, F. A. & Goodgame, D. M. L. (1960). J. Am. Chem. Soc. 82, 5771–5774.

Pinkas, J., Wessel, H., Yang, Y., Monter, M. L., Noltermeye, M., Frolba, M. & Roesky, H. W. (1998). Inorg. Chem. 37, 2450–2457.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Sheldrick, G. M. (2000). SHELXTL. Version 6.10. Bruker AXS Inc., Madison, Wisconsin, USA.

Siemens (1994). SAINT. Siemens Energy and Automation Inc., Madison, Wisconsin, USA.

Siemens (1996). SMART and XPREP. Siemens Energy and Automation Inc., Madison, Wisconsin, USA.

Zeller, A., Herdtweck, E. & Strassner, T. (2001). Acta Cryst. E57, m480–m482.