Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807039700/bt2473sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807039700/bt2473Isup2.hkl |
CCDC reference: 648747
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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).
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%.
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).
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).
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).
Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. |
[Zn(NCS)2(C18H15OP)2] | Z = 4 |
Mr = 738.07 | F(000) = 1520 |
Triclinic, P1 | Dx = 1.358 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.9695 (6) Å | Cell parameters from 22725 reflections |
b = 19.6036 (12) Å | θ = 2.2–28.2° |
c = 21.2407 (12) Å | µ = 0.92 mm−1 |
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 |
Siemens SMART CCD diffractometer | 12513 independent reflections |
Radiation source: fine-focus sealed tube | 10612 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
ω scans | θmax = 25.0°, θmin = 1.1° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.837, Tmax = 0.898 | k = −23→16 |
37146 measured reflections | l = −23→25 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.091 | H-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 parameters | Δρmax = 0.45 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
[Zn(NCS)2(C18H15OP)2] | γ = 95.098 (3)° |
Mr = 738.07 | V = 3610.2 (4) Å3 |
Triclinic, P1 | Z = 4 |
a = 9.9695 (6) Å | Mo Kα radiation |
b = 19.6036 (12) Å | µ = 0.92 mm−1 |
c = 21.2407 (12) Å | T = 298 K |
α = 116.799 (3)° | 0.20 × 0.15 × 0.12 mm |
β = 98.316 (3)° |
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 = 0.898 | Rint = 0.057 |
37146 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.45 e Å−3 |
12513 reflections | Δρmin = −0.48 e Å−3 |
847 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Zn1 | 0.13192 (2) | 1.052920 (13) | 0.847081 (13) | 0.04077 (7) | |
Zn2 | 0.56423 (2) | 0.630566 (14) | 0.368980 (13) | 0.04653 (8) | |
S1 | −0.08062 (8) | 1.26379 (4) | 0.88646 (4) | 0.0737 (2) | |
S2 | 0.45853 (9) | 1.23027 (5) | 1.04395 (5) | 0.0906 (3) | |
S3 | 0.53990 (8) | 0.89535 (4) | 0.48324 (4) | 0.0757 (2) | |
S4 | 0.75445 (13) | 0.51796 (5) | 0.50542 (5) | 0.1086 (4) | |
P1 | 0.25043 (5) | 0.96611 (3) | 0.69865 (3) | 0.04347 (13) | |
P2 | −0.10195 (5) | 0.91425 (3) | 0.83896 (3) | 0.04148 (13) | |
P3 | 0.74093 (5) | 0.62405 (3) | 0.24295 (3) | 0.04247 (13) | |
P4 | 0.31137 (5) | 0.49654 (3) | 0.26626 (3) | 0.04336 (13) | |
O1 | 0.21036 (16) | 0.98176 (9) | 0.76912 (8) | 0.0544 (4) | |
O2 | −0.00785 (17) | 0.98849 (9) | 0.86071 (9) | 0.0616 (4) | |
O3 | 0.65577 (16) | 0.60806 (10) | 0.28875 (9) | 0.0599 (4) | |
O4 | 0.37749 (14) | 0.57989 (8) | 0.31675 (9) | 0.0551 (4) | |
N1 | 0.0359 (2) | 1.13118 (12) | 0.83707 (12) | 0.0614 (5) | |
N2 | 0.2797 (2) | 1.10586 (12) | 0.93108 (11) | 0.0611 (5) | |
N3 | 0.5642 (2) | 0.74096 (13) | 0.41903 (12) | 0.0692 (6) | |
N4 | 0.6444 (3) | 0.58588 (14) | 0.42612 (13) | 0.0782 (7) | |
C1 | −0.0123 (2) | 1.18685 (14) | 0.85828 (12) | 0.0490 (5) | |
C2 | 0.3557 (2) | 1.15767 (13) | 0.97794 (12) | 0.0495 (5) | |
C3 | 0.1311 (2) | 0.99525 (13) | 0.64781 (12) | 0.0489 (5) | |
C4 | 0.1331 (3) | 1.07421 (16) | 0.67189 (17) | 0.0763 (8) | |
H4 | 0.2023 | 1.1103 | 0.7099 | 0.092* | |
C5 | 0.0335 (4) | 1.0991 (2) | 0.6398 (2) | 0.0942 (10) | |
H5 | 0.0361 | 1.1520 | 0.6561 | 0.113* | |
C6 | −0.0686 (3) | 1.0476 (2) | 0.5848 (2) | 0.0893 (10) | |
H6 | −0.1367 | 1.0653 | 0.5642 | 0.107* | |
C7 | −0.0719 (3) | 0.9698 (2) | 0.55953 (19) | 0.0881 (10) | |
H7 | −0.1414 | 0.9345 | 0.5212 | 0.106* | |
C8 | 0.0285 (2) | 0.94324 (17) | 0.59094 (15) | 0.0673 (7) | |
H8 | 0.0264 | 0.8902 | 0.5735 | 0.081* | |
C9 | 0.4192 (2) | 1.01616 (12) | 0.71102 (11) | 0.0460 (5) | |
C10 | 0.5157 (2) | 1.03588 (13) | 0.77341 (13) | 0.0532 (5) | |
H10 | 0.4900 | 1.0277 | 0.8102 | 0.064* | |
C11 | 0.6501 (2) | 1.06763 (14) | 0.78059 (15) | 0.0617 (6) | |
H11 | 0.7143 | 1.0812 | 0.8225 | 0.074* | |
C12 | 0.6893 (2) | 1.07927 (15) | 0.72641 (15) | 0.0632 (7) | |
H12 | 0.7804 | 1.0996 | 0.7312 | 0.076* | |
C13 | 0.5940 (3) | 1.06093 (16) | 0.66515 (14) | 0.0666 (7) | |
H13 | 0.6204 | 1.0696 | 0.6287 | 0.080* | |
C14 | 0.4593 (2) | 1.02972 (15) | 0.65734 (13) | 0.0588 (6) | |
H14 | 0.3951 | 1.0177 | 0.6158 | 0.071* | |
C15 | 0.2511 (2) | 0.86410 (12) | 0.64717 (12) | 0.0454 (5) | |
C16 | 0.3470 (2) | 0.83581 (14) | 0.60491 (14) | 0.0632 (7) | |
H16 | 0.4141 | 0.8703 | 0.6028 | 0.076* | |
C17 | 0.3439 (3) | 0.75717 (16) | 0.56604 (16) | 0.0752 (8) | |
H17 | 0.4090 | 0.7391 | 0.5380 | 0.090* | |
C18 | 0.2457 (3) | 0.70546 (15) | 0.56835 (16) | 0.0699 (7) | |
H18 | 0.2440 | 0.6524 | 0.5421 | 0.084* | |
C19 | 0.1498 (3) | 0.73258 (15) | 0.60967 (17) | 0.0749 (8) | |
H19 | 0.0822 | 0.6976 | 0.6110 | 0.090* | |
C20 | 0.1525 (3) | 0.81102 (14) | 0.64913 (15) | 0.0640 (7) | |
H20 | 0.0875 | 0.8286 | 0.6774 | 0.077* | |
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 | −0.1818 | 0.9435 | 0.7227 | 0.073* | |
C23 | −0.2365 (3) | 0.8456 (2) | 0.62824 (16) | 0.0796 (9) | |
H23 | −0.2648 | 0.8692 | 0.6004 | 0.096* | |
C24 | −0.2433 (3) | 0.7667 (2) | 0.59641 (16) | 0.0851 (10) | |
H24 | −0.2756 | 0.7371 | 0.5469 | 0.102* | |
C25 | −0.2033 (3) | 0.73135 (17) | 0.63665 (15) | 0.0759 (8) | |
H25 | −0.2076 | 0.6778 | 0.6144 | 0.091* | |
C26 | −0.1563 (2) | 0.77469 (13) | 0.71037 (13) | 0.0559 (6) | |
H26 | −0.1303 | 0.7504 | 0.7379 | 0.067* | |
C27 | −0.0242 (2) | 0.85997 (12) | 0.87847 (11) | 0.0457 (5) | |
C28 | 0.1077 (2) | 0.84514 (16) | 0.86907 (14) | 0.0638 (7) | |
H28 | 0.1508 | 0.8608 | 0.8405 | 0.077* | |
C29 | 0.1739 (3) | 0.80750 (18) | 0.90191 (17) | 0.0814 (9) | |
H29 | 0.2618 | 0.7976 | 0.8955 | 0.098* | |
C30 | 0.1110 (4) | 0.78457 (17) | 0.94402 (17) | 0.0841 (9) | |
H30 | 0.1567 | 0.7595 | 0.9665 | 0.101* | |
C31 | −0.0192 (4) | 0.79833 (18) | 0.95330 (17) | 0.0808 (8) | |
H31 | −0.0614 | 0.7824 | 0.9819 | 0.097* | |
C32 | −0.0876 (3) | 0.83564 (15) | 0.92060 (14) | 0.0635 (6) | |
H32 | −0.1761 | 0.8445 | 0.9267 | 0.076* | |
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 | −0.3774 | 0.8302 | 0.7932 | 0.078* | |
C35 | −0.5050 (3) | 0.89542 (16) | 0.85093 (17) | 0.0702 (7) | |
H35 | −0.5845 | 0.8581 | 0.8274 | 0.084* | |
C36 | −0.5110 (3) | 0.96633 (17) | 0.90499 (14) | 0.0627 (7) | |
H36 | −0.5947 | 0.9775 | 0.9180 | 0.075* | |
C37 | −0.3951 (3) | 1.02105 (16) | 0.94019 (14) | 0.0663 (7) | |
H37 | −0.4003 | 1.0694 | 0.9770 | 0.080* | |
C38 | −0.2685 (2) | 1.00533 (14) | 0.92164 (12) | 0.0552 (6) | |
H38 | −0.1894 | 1.0427 | 0.9462 | 0.066* | |
C39 | 0.5547 (2) | 0.80563 (14) | 0.44501 (12) | 0.0509 (5) | |
C40 | 0.6879 (3) | 0.55690 (16) | 0.45897 (14) | 0.0682 (7) | |
C41 | 0.6649 (2) | 0.68279 (12) | 0.20796 (12) | 0.0454 (5) | |
C42 | 0.5521 (3) | 0.71419 (17) | 0.23084 (16) | 0.0727 (8) | |
H42 | 0.5198 | 0.7085 | 0.2675 | 0.087* | |
C43 | 0.4862 (3) | 0.7542 (2) | 0.19961 (19) | 0.0940 (10) | |
H43 | 0.4094 | 0.7748 | 0.2151 | 0.113* | |
C44 | 0.5331 (3) | 0.76350 (16) | 0.14668 (16) | 0.0737 (8) | |
H44 | 0.4873 | 0.7895 | 0.1253 | 0.088* | |
C45 | 0.6471 (3) | 0.73484 (18) | 0.12472 (18) | 0.0776 (8) | |
H45 | 0.6807 | 0.7425 | 0.0894 | 0.093* | |
C46 | 0.7125 (3) | 0.69439 (18) | 0.15505 (17) | 0.0735 (8) | |
H46 | 0.7899 | 0.6746 | 0.1396 | 0.088* | |
C47 | 0.9126 (2) | 0.67214 (13) | 0.29397 (13) | 0.0491 (5) | |
C48 | 0.9381 (3) | 0.69812 (17) | 0.36752 (15) | 0.0719 (7) | |
H48 | 0.8688 | 0.6883 | 0.3889 | 0.086* | |
C49 | 1.0668 (3) | 0.7388 (2) | 0.40967 (19) | 0.0947 (10) | |
H49 | 1.0834 | 0.7565 | 0.4592 | 0.114* | |
C50 | 1.1686 (3) | 0.75293 (18) | 0.3787 (2) | 0.0931 (11) | |
H50 | 1.2549 | 0.7799 | 0.4071 | 0.112* | |
C51 | 1.1447 (3) | 0.72767 (18) | 0.3063 (2) | 0.0865 (10) | |
H51 | 1.2150 | 0.7376 | 0.2856 | 0.104* | |
C52 | 1.0162 (2) | 0.68712 (15) | 0.26282 (16) | 0.0686 (7) | |
H52 | 1.0003 | 0.6703 | 0.2134 | 0.082* | |
C53 | 0.7476 (2) | 0.53510 (12) | 0.16532 (12) | 0.0432 (5) | |
C54 | 0.8561 (3) | 0.49588 (15) | 0.16201 (16) | 0.0683 (7) | |
H54 | 0.9330 | 0.5171 | 0.1996 | 0.082* | |
C55 | 0.8510 (3) | 0.42478 (16) | 0.10277 (19) | 0.0873 (10) | |
H55 | 0.9255 | 0.3989 | 0.1003 | 0.105* | |
C56 | 0.7372 (3) | 0.39215 (15) | 0.04772 (16) | 0.0739 (8) | |
H56 | 0.7343 | 0.3443 | 0.0081 | 0.089* | |
C57 | 0.6274 (3) | 0.43035 (16) | 0.05126 (15) | 0.0728 (7) | |
H57 | 0.5492 | 0.4079 | 0.0144 | 0.087* | |
C58 | 0.6327 (2) | 0.50157 (15) | 0.10901 (14) | 0.0619 (6) | |
H58 | 0.5588 | 0.5277 | 0.1106 | 0.074* | |
C59 | 0.2675 (2) | 0.48219 (14) | 0.17566 (13) | 0.0502 (5) | |
C60 | 0.2558 (3) | 0.54711 (18) | 0.16597 (17) | 0.0772 (8) | |
H60 | 0.2744 | 0.5963 | 0.2057 | 0.093* | |
C61 | 0.2165 (4) | 0.5387 (2) | 0.0977 (2) | 0.1054 (12) | |
H61 | 0.2075 | 0.5823 | 0.0915 | 0.126* | |
C62 | 0.1910 (4) | 0.4678 (3) | 0.0395 (2) | 0.0995 (11) | |
H62 | 0.1653 | 0.4630 | −0.0064 | 0.119* | |
C63 | 0.2026 (3) | 0.4026 (2) | 0.04727 (16) | 0.0835 (9) | |
H63 | 0.1845 | 0.3539 | 0.0069 | 0.100* | |
C64 | 0.2415 (3) | 0.40969 (16) | 0.11559 (14) | 0.0647 (7) | |
H64 | 0.2501 | 0.3657 | 0.1211 | 0.078* | |
C65 | 0.4176 (2) | 0.42756 (12) | 0.26716 (12) | 0.0455 (5) | |
C66 | 0.5101 (2) | 0.40487 (15) | 0.22166 (14) | 0.0626 (6) | |
H66 | 0.5143 | 0.4234 | 0.1885 | 0.075* | |
C67 | 0.5954 (3) | 0.35495 (18) | 0.22573 (16) | 0.0778 (9) | |
H67 | 0.6570 | 0.3393 | 0.1951 | 0.093* | |
C68 | 0.5896 (3) | 0.32809 (15) | 0.27513 (18) | 0.0768 (9) | |
H68 | 0.6457 | 0.2933 | 0.2769 | 0.092* | |
C69 | 0.5016 (3) | 0.35221 (18) | 0.32184 (19) | 0.0788 (9) | |
H69 | 0.5005 | 0.3353 | 0.3563 | 0.095* | |
C70 | 0.4145 (2) | 0.40171 (16) | 0.31761 (16) | 0.0646 (7) | |
H70 | 0.3537 | 0.4176 | 0.3488 | 0.077* | |
C71 | 0.15697 (19) | 0.47608 (12) | 0.29288 (12) | 0.0435 (5) | |
C72 | 0.0756 (2) | 0.40260 (14) | 0.25765 (14) | 0.0582 (6) | |
H72 | 0.0988 | 0.3630 | 0.2180 | 0.070* | |
C73 | −0.0393 (2) | 0.38894 (16) | 0.28186 (16) | 0.0701 (7) | |
H73 | −0.0933 | 0.3397 | 0.2587 | 0.084* | |
C74 | −0.0753 (2) | 0.44714 (17) | 0.33991 (16) | 0.0696 (7) | |
H74 | −0.1531 | 0.4373 | 0.3559 | 0.084* | |
C75 | 0.0033 (3) | 0.51953 (16) | 0.37412 (15) | 0.0697 (7) | |
H75 | −0.0217 | 0.5590 | 0.4132 | 0.084* | |
C76 | 0.1194 (2) | 0.53448 (14) | 0.35106 (13) | 0.0584 (6) | |
H76 | 0.1725 | 0.5839 | 0.3746 | 0.070* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.03915 (12) | 0.03626 (13) | 0.04320 (14) | 0.00350 (9) | 0.00903 (10) | 0.01595 (11) |
Zn2 | 0.04996 (14) | 0.04471 (15) | 0.04040 (14) | 0.00410 (11) | 0.00907 (10) | 0.01699 (12) |
S1 | 0.0772 (4) | 0.0592 (4) | 0.0834 (5) | 0.0265 (3) | 0.0200 (4) | 0.0290 (4) |
S2 | 0.0891 (5) | 0.0618 (4) | 0.0803 (5) | −0.0048 (4) | −0.0310 (4) | 0.0161 (4) |
S3 | 0.0885 (5) | 0.0505 (4) | 0.0766 (5) | 0.0154 (3) | 0.0079 (4) | 0.0225 (4) |
S4 | 0.1950 (11) | 0.0843 (6) | 0.0607 (5) | 0.0675 (6) | 0.0265 (6) | 0.0385 (4) |
P1 | 0.0471 (3) | 0.0440 (3) | 0.0416 (3) | 0.0107 (2) | 0.0150 (2) | 0.0198 (3) |
P2 | 0.0433 (3) | 0.0378 (3) | 0.0433 (3) | 0.0040 (2) | 0.0161 (2) | 0.0175 (2) |
P3 | 0.0393 (3) | 0.0442 (3) | 0.0480 (3) | 0.0103 (2) | 0.0128 (2) | 0.0237 (3) |
P4 | 0.0381 (3) | 0.0402 (3) | 0.0513 (3) | 0.0066 (2) | 0.0111 (2) | 0.0206 (3) |
O1 | 0.0659 (9) | 0.0591 (9) | 0.0481 (9) | 0.0216 (8) | 0.0273 (7) | 0.0272 (8) |
O2 | 0.0674 (10) | 0.0462 (9) | 0.0632 (10) | −0.0080 (7) | 0.0266 (8) | 0.0184 (8) |
O3 | 0.0622 (9) | 0.0656 (10) | 0.0632 (10) | 0.0136 (8) | 0.0291 (8) | 0.0350 (9) |
O4 | 0.0464 (8) | 0.0405 (8) | 0.0686 (11) | 0.0032 (6) | 0.0113 (7) | 0.0183 (8) |
N1 | 0.0599 (12) | 0.0569 (13) | 0.0732 (14) | 0.0161 (10) | 0.0121 (10) | 0.0349 (11) |
N2 | 0.0515 (11) | 0.0559 (12) | 0.0576 (13) | 0.0042 (9) | −0.0009 (9) | 0.0155 (11) |
N3 | 0.0771 (14) | 0.0505 (13) | 0.0616 (14) | 0.0067 (11) | 0.0115 (11) | 0.0123 (11) |
N4 | 0.1013 (18) | 0.0761 (16) | 0.0599 (14) | 0.0168 (13) | 0.0049 (12) | 0.0375 (13) |
C1 | 0.0462 (11) | 0.0522 (14) | 0.0499 (13) | 0.0048 (10) | 0.0054 (9) | 0.0272 (11) |
C2 | 0.0481 (12) | 0.0517 (13) | 0.0497 (13) | 0.0144 (10) | 0.0058 (10) | 0.0250 (12) |
C3 | 0.0500 (12) | 0.0564 (14) | 0.0470 (13) | 0.0125 (10) | 0.0166 (10) | 0.0277 (11) |
C4 | 0.093 (2) | 0.0579 (16) | 0.0744 (19) | 0.0222 (14) | 0.0061 (15) | 0.0295 (15) |
C5 | 0.119 (3) | 0.085 (2) | 0.098 (3) | 0.050 (2) | 0.025 (2) | 0.054 (2) |
C6 | 0.0753 (19) | 0.126 (3) | 0.108 (3) | 0.041 (2) | 0.0258 (19) | 0.084 (3) |
C7 | 0.0593 (16) | 0.121 (3) | 0.092 (2) | −0.0030 (17) | −0.0059 (15) | 0.067 (2) |
C8 | 0.0576 (14) | 0.0720 (17) | 0.0752 (18) | 0.0029 (12) | 0.0040 (13) | 0.0415 (15) |
C9 | 0.0497 (11) | 0.0436 (12) | 0.0422 (12) | 0.0079 (9) | 0.0107 (9) | 0.0177 (10) |
C10 | 0.0613 (13) | 0.0512 (13) | 0.0517 (14) | 0.0093 (11) | 0.0074 (10) | 0.0294 (11) |
C11 | 0.0562 (13) | 0.0604 (15) | 0.0651 (16) | 0.0057 (11) | −0.0060 (11) | 0.0328 (13) |
C12 | 0.0491 (13) | 0.0596 (15) | 0.0751 (18) | 0.0017 (11) | 0.0074 (12) | 0.0298 (14) |
C13 | 0.0651 (15) | 0.0759 (18) | 0.0568 (15) | −0.0043 (13) | 0.0156 (12) | 0.0317 (14) |
C14 | 0.0559 (13) | 0.0706 (16) | 0.0431 (13) | −0.0036 (11) | 0.0051 (10) | 0.0249 (12) |
C15 | 0.0461 (11) | 0.0447 (12) | 0.0470 (12) | 0.0109 (9) | 0.0134 (9) | 0.0215 (10) |
C16 | 0.0613 (14) | 0.0537 (15) | 0.0708 (17) | 0.0101 (12) | 0.0286 (13) | 0.0219 (13) |
C17 | 0.0787 (18) | 0.0626 (17) | 0.0791 (19) | 0.0256 (14) | 0.0353 (15) | 0.0212 (15) |
C18 | 0.0850 (18) | 0.0477 (14) | 0.0730 (18) | 0.0210 (13) | 0.0141 (14) | 0.0239 (13) |
C19 | 0.0836 (18) | 0.0506 (15) | 0.099 (2) | 0.0116 (13) | 0.0307 (16) | 0.0390 (16) |
C20 | 0.0694 (15) | 0.0546 (15) | 0.0822 (18) | 0.0164 (12) | 0.0359 (13) | 0.0374 (14) |
C21 | 0.0405 (10) | 0.0466 (12) | 0.0464 (12) | 0.0056 (9) | 0.0152 (9) | 0.0216 (10) |
C22 | 0.0639 (14) | 0.0674 (16) | 0.0608 (16) | 0.0182 (12) | 0.0163 (12) | 0.0363 (14) |
C23 | 0.0683 (17) | 0.119 (3) | 0.0653 (19) | 0.0128 (17) | 0.0055 (14) | 0.058 (2) |
C24 | 0.0741 (18) | 0.110 (3) | 0.0479 (16) | −0.0131 (17) | 0.0020 (13) | 0.0252 (18) |
C25 | 0.0833 (18) | 0.0594 (16) | 0.0557 (17) | −0.0147 (14) | 0.0171 (14) | 0.0061 (14) |
C26 | 0.0641 (14) | 0.0476 (13) | 0.0499 (14) | −0.0003 (11) | 0.0159 (11) | 0.0183 (11) |
C27 | 0.0459 (11) | 0.0450 (12) | 0.0401 (11) | 0.0056 (9) | 0.0074 (9) | 0.0156 (10) |
C28 | 0.0525 (13) | 0.0711 (17) | 0.0632 (16) | 0.0162 (12) | 0.0123 (11) | 0.0267 (14) |
C29 | 0.0705 (17) | 0.079 (2) | 0.077 (2) | 0.0308 (15) | 0.0024 (15) | 0.0216 (17) |
C30 | 0.109 (2) | 0.0595 (17) | 0.071 (2) | 0.0254 (17) | −0.0117 (17) | 0.0260 (15) |
C31 | 0.105 (2) | 0.0759 (19) | 0.074 (2) | 0.0131 (17) | 0.0124 (16) | 0.0486 (17) |
C32 | 0.0694 (15) | 0.0672 (16) | 0.0666 (17) | 0.0150 (13) | 0.0196 (13) | 0.0403 (14) |
C33 | 0.0491 (11) | 0.0446 (12) | 0.0480 (12) | 0.0134 (9) | 0.0204 (9) | 0.0259 (10) |
C34 | 0.0571 (14) | 0.0488 (14) | 0.0828 (18) | 0.0070 (11) | 0.0305 (13) | 0.0205 (13) |
C35 | 0.0520 (13) | 0.0699 (17) | 0.093 (2) | 0.0097 (12) | 0.0308 (13) | 0.0371 (16) |
C36 | 0.0594 (14) | 0.0856 (19) | 0.0661 (16) | 0.0326 (14) | 0.0321 (13) | 0.0462 (15) |
C37 | 0.0808 (18) | 0.0714 (17) | 0.0512 (15) | 0.0370 (15) | 0.0280 (13) | 0.0243 (13) |
C38 | 0.0621 (13) | 0.0567 (14) | 0.0431 (13) | 0.0164 (11) | 0.0125 (10) | 0.0187 (11) |
C39 | 0.0501 (12) | 0.0543 (15) | 0.0390 (12) | 0.0027 (10) | 0.0028 (9) | 0.0171 (11) |
C40 | 0.096 (2) | 0.0609 (16) | 0.0435 (14) | 0.0212 (14) | 0.0151 (13) | 0.0196 (13) |
C41 | 0.0416 (10) | 0.0417 (11) | 0.0508 (13) | 0.0068 (9) | 0.0069 (9) | 0.0208 (10) |
C42 | 0.0778 (17) | 0.089 (2) | 0.0745 (18) | 0.0469 (15) | 0.0340 (14) | 0.0474 (17) |
C43 | 0.097 (2) | 0.113 (3) | 0.100 (3) | 0.071 (2) | 0.0377 (19) | 0.060 (2) |
C44 | 0.0880 (19) | 0.0561 (16) | 0.0742 (19) | 0.0235 (14) | −0.0021 (15) | 0.0317 (14) |
C45 | 0.0848 (19) | 0.083 (2) | 0.095 (2) | 0.0217 (16) | 0.0236 (16) | 0.0648 (19) |
C46 | 0.0600 (15) | 0.094 (2) | 0.104 (2) | 0.0303 (14) | 0.0314 (14) | 0.0713 (19) |
C47 | 0.0438 (11) | 0.0442 (12) | 0.0569 (14) | 0.0115 (9) | 0.0054 (10) | 0.0225 (11) |
C48 | 0.0633 (15) | 0.0818 (19) | 0.0647 (18) | 0.0117 (14) | −0.0010 (13) | 0.0338 (16) |
C49 | 0.078 (2) | 0.100 (3) | 0.077 (2) | 0.0189 (18) | −0.0169 (17) | 0.0258 (19) |
C50 | 0.0553 (17) | 0.0660 (19) | 0.118 (3) | 0.0117 (14) | −0.0196 (18) | 0.020 (2) |
C51 | 0.0489 (14) | 0.0704 (19) | 0.122 (3) | 0.0043 (13) | 0.0158 (16) | 0.031 (2) |
C52 | 0.0488 (13) | 0.0664 (16) | 0.0800 (19) | 0.0044 (12) | 0.0148 (12) | 0.0261 (15) |
C53 | 0.0430 (10) | 0.0407 (11) | 0.0502 (12) | 0.0076 (9) | 0.0137 (9) | 0.0240 (10) |
C54 | 0.0527 (13) | 0.0528 (14) | 0.0847 (19) | 0.0175 (11) | 0.0038 (12) | 0.0214 (14) |
C55 | 0.0745 (18) | 0.0554 (16) | 0.112 (3) | 0.0314 (14) | 0.0181 (17) | 0.0197 (17) |
C56 | 0.093 (2) | 0.0468 (14) | 0.0705 (18) | 0.0160 (14) | 0.0227 (15) | 0.0154 (13) |
C57 | 0.0779 (17) | 0.0609 (16) | 0.0580 (16) | 0.0058 (14) | 0.0012 (13) | 0.0146 (14) |
C58 | 0.0554 (13) | 0.0632 (16) | 0.0614 (16) | 0.0173 (12) | 0.0089 (11) | 0.0243 (13) |
C59 | 0.0450 (11) | 0.0573 (14) | 0.0575 (14) | 0.0143 (10) | 0.0170 (10) | 0.0320 (12) |
C60 | 0.107 (2) | 0.0699 (18) | 0.080 (2) | 0.0374 (16) | 0.0399 (17) | 0.0475 (16) |
C61 | 0.158 (4) | 0.112 (3) | 0.099 (3) | 0.065 (3) | 0.055 (3) | 0.079 (3) |
C62 | 0.115 (3) | 0.142 (3) | 0.077 (2) | 0.049 (2) | 0.0295 (19) | 0.074 (3) |
C63 | 0.087 (2) | 0.100 (2) | 0.0570 (18) | 0.0140 (17) | 0.0092 (14) | 0.0334 (17) |
C64 | 0.0663 (15) | 0.0667 (17) | 0.0602 (16) | 0.0082 (12) | 0.0073 (12) | 0.0315 (14) |
C65 | 0.0373 (10) | 0.0402 (11) | 0.0520 (13) | 0.0034 (8) | 0.0054 (9) | 0.0175 (10) |
C66 | 0.0537 (13) | 0.0730 (17) | 0.0541 (15) | 0.0207 (12) | 0.0099 (11) | 0.0226 (13) |
C67 | 0.0581 (15) | 0.086 (2) | 0.0677 (18) | 0.0342 (14) | 0.0072 (13) | 0.0158 (16) |
C68 | 0.0541 (15) | 0.0528 (15) | 0.104 (2) | 0.0150 (12) | −0.0092 (15) | 0.0267 (16) |
C69 | 0.0578 (15) | 0.084 (2) | 0.121 (3) | 0.0120 (14) | 0.0068 (16) | 0.074 (2) |
C70 | 0.0509 (13) | 0.0769 (18) | 0.0868 (19) | 0.0169 (12) | 0.0212 (12) | 0.0533 (16) |
C71 | 0.0379 (10) | 0.0458 (12) | 0.0489 (12) | 0.0094 (9) | 0.0093 (9) | 0.0236 (10) |
C72 | 0.0481 (12) | 0.0481 (13) | 0.0688 (16) | 0.0060 (10) | 0.0183 (11) | 0.0181 (12) |
C73 | 0.0513 (13) | 0.0574 (15) | 0.093 (2) | −0.0023 (11) | 0.0189 (13) | 0.0294 (15) |
C74 | 0.0483 (13) | 0.0816 (19) | 0.0813 (19) | 0.0057 (13) | 0.0248 (13) | 0.0382 (17) |
C75 | 0.0633 (15) | 0.0737 (18) | 0.0640 (16) | 0.0120 (13) | 0.0295 (13) | 0.0206 (14) |
C76 | 0.0526 (13) | 0.0536 (14) | 0.0569 (15) | 0.0033 (11) | 0.0135 (11) | 0.0162 (12) |
Zn1—N2 | 1.931 (2) | C30—C31 | 1.373 (5) |
Zn1—O2 | 1.9376 (15) | C30—H30 | 0.9300 |
Zn1—O1 | 1.9454 (15) | C31—C32 | 1.375 (4) |
Zn1—N1 | 1.952 (2) | C31—H31 | 0.9300 |
Zn2—N4 | 1.919 (2) | C32—H32 | 0.9300 |
Zn2—N3 | 1.934 (2) | C33—C38 | 1.378 (3) |
Zn2—O4 | 1.9400 (14) | C33—C34 | 1.388 (3) |
Zn2—O3 | 1.9429 (15) | C34—C35 | 1.388 (3) |
S1—C1 | 1.607 (3) | C34—H34 | 0.9300 |
S2—C2 | 1.603 (2) | C35—C36 | 1.360 (4) |
S3—C39 | 1.602 (3) | C35—H35 | 0.9300 |
S4—C40 | 1.605 (3) | C36—C37 | 1.360 (4) |
P1—O1 | 1.5084 (15) | C36—H36 | 0.9300 |
P1—C9 | 1.792 (2) | C37—C38 | 1.395 (3) |
P1—C3 | 1.792 (2) | C37—H37 | 0.9300 |
P1—C15 | 1.797 (2) | C38—H38 | 0.9300 |
P2—O2 | 1.4959 (15) | C41—C42 | 1.375 (3) |
P2—C27 | 1.789 (2) | C41—C46 | 1.380 (3) |
P2—C33 | 1.793 (2) | C42—C43 | 1.386 (4) |
P2—C21 | 1.793 (2) | C42—H42 | 0.9300 |
P3—O3 | 1.4939 (16) | C43—C44 | 1.355 (4) |
P3—C41 | 1.793 (2) | C43—H43 | 0.9300 |
P3—C53 | 1.795 (2) | C44—C45 | 1.362 (4) |
P3—C47 | 1.802 (2) | C44—H44 | 0.9300 |
P4—O4 | 1.5095 (15) | C45—C46 | 1.378 (4) |
P4—C71 | 1.788 (2) | C45—H45 | 0.9300 |
P4—C59 | 1.795 (2) | C46—H46 | 0.9300 |
P4—C65 | 1.795 (2) | C47—C48 | 1.382 (4) |
N1—C1 | 1.157 (3) | C47—C52 | 1.382 (3) |
N2—C2 | 1.153 (3) | C48—C49 | 1.388 (4) |
N3—C39 | 1.152 (3) | C48—H48 | 0.9300 |
N4—C40 | 1.145 (3) | C49—C50 | 1.359 (5) |
C3—C8 | 1.375 (3) | C49—H49 | 0.9300 |
C3—C4 | 1.391 (3) | C50—C51 | 1.362 (5) |
C4—C5 | 1.370 (4) | C50—H50 | 0.9300 |
C4—H4 | 0.9300 | C51—C52 | 1.393 (4) |
C5—C6 | 1.352 (5) | C51—H51 | 0.9300 |
C5—H5 | 0.9300 | C52—H52 | 0.9300 |
C6—C7 | 1.366 (5) | C53—C54 | 1.374 (3) |
C6—H6 | 0.9300 | C53—C58 | 1.391 (3) |
C7—C8 | 1.389 (4) | C54—C55 | 1.384 (4) |
C7—H7 | 0.9300 | C54—H54 | 0.9300 |
C8—H8 | 0.9300 | C55—C56 | 1.370 (4) |
C9—C14 | 1.384 (3) | C55—H55 | 0.9300 |
C9—C10 | 1.391 (3) | C56—C57 | 1.372 (4) |
C10—C11 | 1.383 (3) | C56—H56 | 0.9300 |
C10—H10 | 0.9300 | C57—C58 | 1.371 (4) |
C11—C12 | 1.372 (4) | C57—H57 | 0.9300 |
C11—H11 | 0.9300 | C58—H58 | 0.9300 |
C12—C13 | 1.373 (4) | C59—C64 | 1.385 (3) |
C12—H12 | 0.9300 | C59—C60 | 1.390 (3) |
C13—C14 | 1.380 (3) | C60—C61 | 1.377 (5) |
C13—H13 | 0.9300 | C60—H60 | 0.9300 |
C14—H14 | 0.9300 | C61—C62 | 1.350 (5) |
C15—C16 | 1.385 (3) | C61—H61 | 0.9300 |
C15—C20 | 1.386 (3) | C62—C63 | 1.372 (5) |
C16—C17 | 1.377 (3) | C62—H62 | 0.9300 |
C16—H16 | 0.9300 | C63—C64 | 1.386 (4) |
C17—C18 | 1.367 (4) | C63—H63 | 0.9300 |
C17—H17 | 0.9300 | C64—H64 | 0.9300 |
C18—C19 | 1.371 (4) | C65—C70 | 1.379 (3) |
C18—H18 | 0.9300 | C65—C66 | 1.387 (3) |
C19—C20 | 1.375 (4) | C66—C67 | 1.375 (4) |
C19—H19 | 0.9300 | C66—H66 | 0.9300 |
C20—H20 | 0.9300 | C67—C68 | 1.376 (4) |
C21—C26 | 1.385 (3) | C67—H67 | 0.9300 |
C21—C22 | 1.389 (3) | C68—C69 | 1.371 (4) |
C22—C23 | 1.374 (4) | C68—H68 | 0.9300 |
C22—H22 | 0.9300 | C69—C70 | 1.382 (4) |
C23—C24 | 1.371 (4) | C69—H69 | 0.9300 |
C23—H23 | 0.9300 | C70—H70 | 0.9300 |
C24—C25 | 1.362 (4) | C71—C76 | 1.383 (3) |
C24—H24 | 0.9300 | C71—C72 | 1.392 (3) |
C25—C26 | 1.382 (4) | C72—C73 | 1.374 (3) |
C25—H25 | 0.9300 | C72—H72 | 0.9300 |
C26—H26 | 0.9300 | C73—C74 | 1.372 (4) |
C27—C32 | 1.387 (3) | C73—H73 | 0.9300 |
C27—C28 | 1.394 (3) | C74—C75 | 1.365 (4) |
C28—C29 | 1.373 (4) | C74—H74 | 0.9300 |
C28—H28 | 0.9300 | C75—C76 | 1.378 (3) |
C29—C30 | 1.368 (5) | C75—H75 | 0.9300 |
C29—H29 | 0.9300 | C76—H76 | 0.9300 |
N2—Zn1—O2 | 111.57 (9) | C32—C31—H31 | 119.8 |
N2—Zn1—O1 | 106.88 (8) | C31—C32—C27 | 119.8 (3) |
O2—Zn1—O1 | 105.69 (7) | C31—C32—H32 | 120.1 |
N2—Zn1—N1 | 107.80 (9) | C27—C32—H32 | 120.1 |
O2—Zn1—N1 | 103.88 (8) | C38—C33—C34 | 119.7 (2) |
O1—Zn1—N1 | 120.98 (8) | C38—C33—P2 | 119.87 (17) |
N4—Zn2—N3 | 116.34 (10) | C34—C33—P2 | 120.35 (17) |
N4—Zn2—O4 | 113.40 (9) | C35—C34—C33 | 119.7 (2) |
N3—Zn2—O4 | 107.47 (8) | C35—C34—H34 | 120.2 |
N4—Zn2—O3 | 109.50 (9) | C33—C34—H34 | 120.2 |
N3—Zn2—O3 | 108.76 (9) | C36—C35—C34 | 120.3 (2) |
O4—Zn2—O3 | 100.07 (7) | C36—C35—H35 | 119.8 |
O1—P1—C9 | 112.56 (10) | C34—C35—H35 | 119.8 |
O1—P1—C3 | 110.67 (9) | C35—C36—C37 | 120.3 (2) |
C9—P1—C3 | 107.94 (10) | C35—C36—H36 | 119.8 |
O1—P1—C15 | 109.13 (10) | C37—C36—H36 | 119.8 |
C9—P1—C15 | 107.21 (10) | C36—C37—C38 | 120.6 (2) |
C3—P1—C15 | 109.24 (11) | C36—C37—H37 | 119.7 |
O2—P2—C27 | 110.57 (10) | C38—C37—H37 | 119.7 |
O2—P2—C33 | 110.33 (10) | C33—C38—C37 | 119.3 (2) |
C27—P2—C33 | 109.39 (10) | C33—C38—H38 | 120.4 |
O2—P2—C21 | 112.59 (10) | C37—C38—H38 | 120.4 |
C27—P2—C21 | 108.77 (10) | N3—C39—S3 | 178.2 (2) |
C33—P2—C21 | 105.01 (10) | N4—C40—S4 | 177.9 (3) |
O3—P3—C41 | 111.22 (10) | C42—C41—C46 | 118.2 (2) |
O3—P3—C53 | 110.14 (10) | C42—C41—P3 | 120.25 (19) |
C41—P3—C53 | 105.46 (10) | C46—C41—P3 | 121.46 (17) |
O3—P3—C47 | 110.51 (11) | C41—C42—C43 | 120.4 (3) |
C41—P3—C47 | 109.37 (10) | C41—C42—H42 | 119.8 |
C53—P3—C47 | 110.01 (10) | C43—C42—H42 | 119.8 |
O4—P4—C71 | 108.46 (9) | C44—C43—C42 | 120.4 (3) |
O4—P4—C59 | 110.00 (10) | C44—C43—H43 | 119.8 |
C71—P4—C59 | 108.65 (10) | C42—C43—H43 | 119.8 |
O4—P4—C65 | 113.75 (9) | C43—C44—C45 | 120.2 (3) |
C71—P4—C65 | 107.38 (10) | C43—C44—H44 | 119.9 |
C59—P4—C65 | 108.46 (11) | C45—C44—H44 | 119.9 |
P1—O1—Zn1 | 144.35 (10) | C44—C45—C46 | 119.8 (3) |
P2—O2—Zn1 | 153.74 (11) | C44—C45—H45 | 120.1 |
P3—O3—Zn2 | 157.78 (11) | C46—C45—H45 | 120.1 |
P4—O4—Zn2 | 133.60 (9) | C45—C46—C41 | 121.0 (2) |
C1—N1—Zn1 | 154.5 (2) | C45—C46—H46 | 119.5 |
C2—N2—Zn1 | 157.2 (2) | C41—C46—H46 | 119.5 |
C39—N3—Zn2 | 174.6 (2) | C48—C47—C52 | 119.4 (2) |
C40—N4—Zn2 | 177.3 (3) | C48—C47—P3 | 118.05 (19) |
N1—C1—S1 | 179.1 (2) | C52—C47—P3 | 122.4 (2) |
N2—C2—S2 | 178.8 (2) | C47—C48—C49 | 120.2 (3) |
C8—C3—C4 | 118.6 (2) | C47—C48—H48 | 119.9 |
C8—C3—P1 | 122.65 (19) | C49—C48—H48 | 119.9 |
C4—C3—P1 | 118.35 (19) | C50—C49—C48 | 120.1 (3) |
C5—C4—C3 | 120.3 (3) | C50—C49—H49 | 119.9 |
C5—C4—H4 | 119.9 | C48—C49—H49 | 119.9 |
C3—C4—H4 | 119.9 | C49—C50—C51 | 120.2 (3) |
C6—C5—C4 | 120.8 (3) | C49—C50—H50 | 119.9 |
C6—C5—H5 | 119.6 | C51—C50—H50 | 119.9 |
C4—C5—H5 | 119.6 | C50—C51—C52 | 120.8 (3) |
C5—C6—C7 | 120.1 (3) | C50—C51—H51 | 119.6 |
C5—C6—H6 | 119.9 | C52—C51—H51 | 119.6 |
C7—C6—H6 | 119.9 | C47—C52—C51 | 119.2 (3) |
C6—C7—C8 | 120.1 (3) | C47—C52—H52 | 120.4 |
C6—C7—H7 | 120.0 | C51—C52—H52 | 120.4 |
C8—C7—H7 | 120.0 | C54—C53—C58 | 118.9 (2) |
C3—C8—C7 | 120.1 (3) | C54—C53—P3 | 122.70 (18) |
C3—C8—H8 | 119.9 | C58—C53—P3 | 118.14 (16) |
C7—C8—H8 | 119.9 | C53—C54—C55 | 120.0 (2) |
C14—C9—C10 | 119.2 (2) | C53—C54—H54 | 120.0 |
C14—C9—P1 | 121.45 (17) | C55—C54—H54 | 120.0 |
C10—C9—P1 | 119.15 (17) | C56—C55—C54 | 120.6 (2) |
C11—C10—C9 | 119.8 (2) | C56—C55—H55 | 119.7 |
C11—C10—H10 | 120.1 | C54—C55—H55 | 119.7 |
C9—C10—H10 | 120.1 | C55—C56—C57 | 119.7 (3) |
C12—C11—C10 | 120.5 (2) | C55—C56—H56 | 120.1 |
C12—C11—H11 | 119.7 | C57—C56—H56 | 120.1 |
C10—C11—H11 | 119.7 | C58—C57—C56 | 120.1 (3) |
C11—C12—C13 | 119.9 (2) | C58—C57—H57 | 119.9 |
C11—C12—H12 | 120.1 | C56—C57—H57 | 119.9 |
C13—C12—H12 | 120.1 | C57—C58—C53 | 120.6 (2) |
C12—C13—C14 | 120.3 (2) | C57—C58—H58 | 119.7 |
C12—C13—H13 | 119.8 | C53—C58—H58 | 119.7 |
C14—C13—H13 | 119.8 | C64—C59—C60 | 118.9 (2) |
C13—C14—C9 | 120.3 (2) | C64—C59—P4 | 123.14 (18) |
C13—C14—H14 | 119.9 | C60—C59—P4 | 117.9 (2) |
C9—C14—H14 | 119.9 | C61—C60—C59 | 120.1 (3) |
C16—C15—C20 | 118.1 (2) | C61—C60—H60 | 120.0 |
C16—C15—P1 | 122.48 (17) | C59—C60—H60 | 120.0 |
C20—C15—P1 | 119.43 (17) | C62—C61—C60 | 120.5 (3) |
C17—C16—C15 | 120.8 (2) | C62—C61—H61 | 119.8 |
C17—C16—H16 | 119.6 | C60—C61—H61 | 119.8 |
C15—C16—H16 | 119.6 | C61—C62—C63 | 120.8 (3) |
C18—C17—C16 | 120.5 (2) | C61—C62—H62 | 119.6 |
C18—C17—H17 | 119.7 | C63—C62—H62 | 119.6 |
C16—C17—H17 | 119.7 | C62—C63—C64 | 119.7 (3) |
C17—C18—C19 | 119.4 (3) | C62—C63—H63 | 120.2 |
C17—C18—H18 | 120.3 | C64—C63—H63 | 120.2 |
C19—C18—H18 | 120.3 | C59—C64—C63 | 120.0 (3) |
C18—C19—C20 | 120.6 (3) | C59—C64—H64 | 120.0 |
C18—C19—H19 | 119.7 | C63—C64—H64 | 120.0 |
C20—C19—H19 | 119.7 | C70—C65—C66 | 119.8 (2) |
C19—C20—C15 | 120.7 (2) | C70—C65—P4 | 119.25 (18) |
C19—C20—H20 | 119.7 | C66—C65—P4 | 120.71 (19) |
C15—C20—H20 | 119.7 | C67—C66—C65 | 119.8 (3) |
C26—C21—C22 | 119.5 (2) | C67—C66—H66 | 120.1 |
C26—C21—P2 | 122.59 (18) | C65—C66—H66 | 120.1 |
C22—C21—P2 | 117.70 (17) | C66—C67—C68 | 120.0 (3) |
C23—C22—C21 | 120.0 (3) | C66—C67—H67 | 120.0 |
C23—C22—H22 | 120.0 | C68—C67—H67 | 120.0 |
C21—C22—H22 | 120.0 | C69—C68—C67 | 120.5 (3) |
C24—C23—C22 | 120.0 (3) | C69—C68—H68 | 119.7 |
C24—C23—H23 | 120.0 | C67—C68—H68 | 119.7 |
C22—C23—H23 | 120.0 | C68—C69—C70 | 119.8 (3) |
C25—C24—C23 | 120.6 (3) | C68—C69—H69 | 120.1 |
C25—C24—H24 | 119.7 | C70—C69—H69 | 120.1 |
C23—C24—H24 | 119.7 | C65—C70—C69 | 120.0 (3) |
C24—C25—C26 | 120.3 (3) | C65—C70—H70 | 120.0 |
C24—C25—H25 | 119.9 | C69—C70—H70 | 120.0 |
C26—C25—H25 | 119.9 | C76—C71—C72 | 119.3 (2) |
C25—C26—C21 | 119.7 (3) | C76—C71—P4 | 118.95 (16) |
C25—C26—H26 | 120.2 | C72—C71—P4 | 121.74 (17) |
C21—C26—H26 | 120.2 | C73—C72—C71 | 119.6 (2) |
C32—C27—C28 | 119.3 (2) | C73—C72—H72 | 120.2 |
C32—C27—P2 | 122.37 (17) | C71—C72—H72 | 120.2 |
C28—C27—P2 | 118.28 (18) | C74—C73—C72 | 120.7 (2) |
C29—C28—C27 | 120.0 (3) | C74—C73—H73 | 119.7 |
C29—C28—H28 | 120.0 | C72—C73—H73 | 119.7 |
C27—C28—H28 | 120.0 | C75—C74—C73 | 120.0 (2) |
C30—C29—C28 | 120.2 (3) | C75—C74—H74 | 120.0 |
C30—C29—H29 | 119.9 | C73—C74—H74 | 120.0 |
C28—C29—H29 | 119.9 | C74—C75—C76 | 120.4 (2) |
C29—C30—C31 | 120.4 (3) | C74—C75—H75 | 119.8 |
C29—C30—H30 | 119.8 | C76—C75—H75 | 119.8 |
C31—C30—H30 | 119.8 | C75—C76—C71 | 120.1 (2) |
C30—C31—C32 | 120.4 (3) | C75—C76—H76 | 120.0 |
C30—C31—H31 | 119.8 | C71—C76—H76 | 120.0 |
Experimental details
Crystal data | |
Chemical formula | [Zn(NCS)2(C18H15OP)2] |
Mr | 738.07 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 3610.2 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.92 |
Crystal size (mm) | 0.20 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Siemens SMART CCD |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.837, 0.898 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 37146, 12513, 10612 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.091, 1.07 |
No. of reflections | 12513 |
No. of parameters | 847 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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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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.