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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807039700/bt2473sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807039700/bt2473Isup2.hkl
Contains datablock I

CCDC reference: 648747

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.032
  • wR factor = 0.090
  • Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for S2 - C2 .. 7.87 su
Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 300 Deg. PLAT230_ALERT_2_C Hirshfeld Test Diff for S1 - C1 .. 5.34 su PLAT230_ALERT_2_C Hirshfeld Test Diff for S3 - C39 .. 5.41 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N4 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C43 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C55 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C61 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zn1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zn2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C39 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C40 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C41
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 2.15 PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn2 (2) 2.20
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 18 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check

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).

Structure description 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.

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).

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
[Zn(NCS)2(C18H15OP)2]Z = 4
Mr = 738.07F(000) = 1520
Triclinic, P1Dx = 1.358 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.9695 (6) ÅCell parameters from 22725 reflections
b = 19.6036 (12) Åθ = 2.2–28.2°
c = 21.2407 (12) ŵ = 0.92 mm1
α = 116.799 (3)°T = 298 K
β = 98.316 (3)°Block, yellow
γ = 95.098 (3)°0.20 × 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)
Graphite monochromatorRint = 0.057
ω scansθmax = 25.0°, θmin = 1.1°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.837, Tmax = 0.898k = 2316
37146 measured reflectionsl = 2325
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0405P)2 + 0.9616P]
where P = (Fo2 + 2Fc2)/3
12513 reflections(Δ/σ)max = 0.001
847 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.48 e Å3
Crystal data top
[Zn(NCS)2(C18H15OP)2]γ = 95.098 (3)°
Mr = 738.07V = 3610.2 (4) Å3
Triclinic, P1Z = 4
a = 9.9695 (6) ÅMo Kα radiation
b = 19.6036 (12) ŵ = 0.92 mm1
c = 21.2407 (12) ÅT = 298 K
α = 116.799 (3)°0.20 × 0.15 × 0.12 mm
β = 98.316 (3)°
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)] = 0.0320 restraints
wR(F2) = 0.091H-atom parameters constrained
S = 1.07Δρmax = 0.45 e Å3
12513 reflectionsΔρmin = 0.48 e Å3
847 parameters
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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)
S10.08062 (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)
P20.10195 (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)
O20.00785 (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)
C10.0123 (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*
C60.0686 (3)1.0476 (2)0.5848 (2)0.0893 (10)
H60.13671.06530.56420.107*
C70.0719 (3)0.9698 (2)0.55953 (19)0.0881 (10)
H70.14140.93450.52120.106*
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*
C210.1479 (2)0.85453 (12)0.74305 (11)0.0441 (5)
C220.1879 (2)0.88990 (16)0.70127 (14)0.0608 (6)
H220.18180.94350.72270.073*
C230.2365 (3)0.8456 (2)0.62824 (16)0.0796 (9)
H230.26480.86920.60040.096*
C240.2433 (3)0.7667 (2)0.59641 (16)0.0851 (10)
H240.27560.73710.54690.102*
C250.2033 (3)0.73135 (17)0.63665 (15)0.0759 (8)
H250.20760.67780.61440.091*
C260.1563 (2)0.77469 (13)0.71037 (13)0.0559 (6)
H260.13030.75040.73790.067*
C270.0242 (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*
C310.0192 (4)0.79833 (18)0.95330 (17)0.0808 (8)
H310.06140.78240.98190.097*
C320.0876 (3)0.83564 (15)0.92060 (14)0.0635 (6)
H320.17610.84450.92670.076*
C330.2620 (2)0.93378 (12)0.86656 (12)0.0441 (5)
C340.3809 (2)0.87841 (14)0.83064 (15)0.0653 (7)
H340.37740.83020.79320.078*
C350.5050 (3)0.89542 (16)0.85093 (17)0.0702 (7)
H350.58450.85810.82740.084*
C360.5110 (3)0.96633 (17)0.90499 (14)0.0627 (7)
H360.59470.97750.91800.075*
C370.3951 (3)1.02105 (16)0.94019 (14)0.0663 (7)
H370.40031.06940.97700.080*
C380.2685 (2)1.00533 (14)0.92164 (12)0.0552 (6)
H380.18941.04270.94620.066*
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)
H620.16530.46300.00640.119*
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*
C730.0393 (2)0.38894 (16)0.28186 (16)0.0701 (7)
H730.09330.33970.25870.084*
C740.0753 (2)0.44714 (17)0.33991 (16)0.0696 (7)
H740.15310.43730.35590.084*
C750.0033 (3)0.51953 (16)0.37412 (15)0.0697 (7)
H750.02170.55900.41320.084*
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, º) 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

Experimental details

Crystal data
Chemical formula[Zn(NCS)2(C18H15OP)2]
Mr738.07
Crystal system, space groupTriclinic, P1
Temperature (K)298
a, b, c (Å)9.9695 (6), 19.6036 (12), 21.2407 (12)
α, β, γ (°)116.799 (3), 98.316 (3), 95.098 (3)
V3)3610.2 (4)
Z4
Radiation typeMo Kα
µ (mm1)0.92
Crystal size (mm)0.20 × 0.15 × 0.12
Data collection
DiffractometerSiemens SMART CCD
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.837, 0.898
No. of measured, independent and
observed [I > 2σ(I)] reflections
37146, 12513, 10612
Rint0.057
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.091, 1.07
No. of reflections12513
No. of parameters847
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.45, 0.48

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), XPREP (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 2000).

 

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