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The Zn atom in the polymeric title complex, [Zn(C12H22O2PS2)2(C12H10N4)]n, lies on a twofold axis and exists in a distorted octa­hedral geometry defined by a cis-N2O4 donor set, provided by two S,S-chelating dithio­phosphate ligands and two N atoms derived from two bridging dipyridyl-type ligands, each of which is disposed about a centre of inversion. The resultant polymeric structure has a zigzag topology.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805029466/ng6201sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805029466/ng6201Isup2.hkl
Contains datablock I

CCDC reference: 287669

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in main residue
  • R factor = 0.057
  • wR factor = 0.137
  • Data-to-parameter ratio = 24.3

checkCIF/PLATON results

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Alert level C PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89 PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 4.00 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.54 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C6 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 C4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C4' PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.29 PLAT301_ALERT_3_C Main Residue Disorder ......................... 12.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

Interest in crystal structures related to the polymeric title complex, [Zn{S2P(OCy)2}2{4-NC5H4C(H)NNC(H)C5H4N-4}]n, (I), arises from the desire to rationalize the formation of polymer topologies based on the steric requirements of the respective ligands, i.e. dithiolate-bound R groups and/or the dipyridyl-type ligands themselves (Lai et al., 2002, 2004a; Tiekink, 2003; Lai & Tiekink, 2004).

The immediate coordination geometry about the Zn atom (Fig. 1) is defined by four S atoms, derived from two chelating dithiophosphate ligands, and two N atoms, derived from two µ2-bridging dipyridyl-type ligands. There is crystallographic symmetry in the structure so that the Zn atom is located on a twofold axis and each dipyridyl-type ligand is disposed about a centre of inversion. The cis-N2S4 donor set defines an octahedral geometry with the major distortion being due to the restricted bite distance of the dithiophosphate ligand, i.e. the S1—Zn—S2 chelate angle is 79.17 (2)°. Other geometric parameters are as expected (Table 1).

The cis disposition of the N-donor atoms gives rise to a polymer with a zigzag topology (Fig. 2). The polymer is aligned along the c axis and a small twist in the dipyridyl-type ligand is noted, as seen in the N2—C18—C15—C16 torsion angle of 19.8 (4)°. It is noteworthy that in the absence of any obvious steric hindrance in the structure of (I), a zigzag polymer is found, an observation consistent with the majority of structures of the general formula [Zn{S2P(OR)2}2(bridging dipyridyl-type ligand)]n. Thus, for each of the [Zn{S2P(OR)2}2(4-NC5H4C5H4N-4)]n, for R = Et (Zhu et al., 1996) and R = iPr (Glinskaya et al., 2000), and [Zn{S2P(OR)2}2(4-NC5H4CH2CH2C5H4N-4)]n, R = iPr and Cy (Lai et al., 2004a) structures, a zigzag topology is found. By contrast, in the two cases where steric influences become a factor in polymer formation, a linear chain is formed, i.e. [Zn{S2P(OCy)2}2{4-NC5H4C(H)C(H)C5H4N-4}]n (Lai et al., 2004a) and [Zn{S2P(OiBu)2}2(4-NC5H4CH2CH2C5H4N-4)]n (Lai et al., 2004b).

Experimental top

The title compound was prepared by refluxing the parent zinc dithiophosphate with 4-pyridinealdazine (Aldrich) using a literature procedure (Lai et al., 2004a). Colourless crystals were isolated in 65% yield by slow evaporation of a chloroform–acetonitrile (3:1 (v/v) solution of the compound (m.p. 377–379 K). Analysis found: C 50.38, H 6.34%; C36H54N4O4P2S4Zn requires: C 50.14, H 6.31%. IR (KBr disk): ν(C—O) 1153 (m), ν(P—O) 968 (s), ν(P—S)asymm 658 (m), ν(P—S)symm 523 (m) cm−1.

Refinement top

H atoms were included in the riding-model approximation, with aromatic C—H = 0.94 Å, methine C—H = 0.99 Å and methylene C—H = 0.98 Å, and with Uiso(H) = 1.2Ueq(C). The C1–C6 cyclohexyl group was disordered and two sites were discerned for atoms C5 and C6. As the occupancy for each site refined to nearly 50%, the occupancies of the disordered atoms were fixed at 50%.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The octahedral coordination geometry for zinc in (I), showing the crystallographic numbering scheme. Displacement ellipsoids are shown at the 50% probability level. Only one position for each of the disordered C5 and C6 atoms is shown. [Symmetry codes: (i) 1 − x, y, 3/2 − z; (ii) 1 − x, 2 − y, 1 − z.]
[Figure 2] Fig. 2. A portion of the zigzag polymer (DIAMOND; Crystal Impact, 2002). Colour code: Zn cyan, S yellow, P pink, O red, N blue, C grey and H green.
catena-Poly[[bis(O,O'-dicyclohexyl dithiophosphato-κ2,S,S')zinc(II)]- µ-1,2-bis(4-pyridylmethylene)hydrazine-κ2N:N'] top
Crystal data top
[Zn(C12H22O2PS2)2(C12H10N4)]Dx = 1.356 Mg m3
Mr = 862.38Melting point = 377–379 K
Orthorhombic, PbcnMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2n 2abCell parameters from 6234 reflections
a = 18.3340 (8) Åθ = 2.4–25.8°
b = 12.0404 (5) ŵ = 0.90 mm1
c = 19.1304 (8) ÅT = 223 K
V = 4223.0 (3) Å3Block, yellow
Z = 40.52 × 0.36 × 0.26 mm
F(000) = 1816
Data collection top
Bruker SMART area-detector
diffractometer
6155 independent reflections
Radiation source: medium-focus sealed tube4886 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
ϕ and ω scansθmax = 30.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS, Bruker, 2000)
h = 2525
Tmin = 0.565, Tmax = 0.792k = 1416
39717 measured reflectionsl = 2626
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)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-atom parameters constrained
S = 1.10 w = 1/[σ2(Fo2) + (0.0635P)2 + 1.9949P]
where P = (Fo2 + 2Fc2)/3
6155 reflections(Δ/σ)max < 0.001
253 parametersΔρmax = 0.92 e Å3
0 restraintsΔρmin = 0.23 e Å3
Crystal data top
[Zn(C12H22O2PS2)2(C12H10N4)]V = 4223.0 (3) Å3
Mr = 862.38Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 18.3340 (8) ŵ = 0.90 mm1
b = 12.0404 (5) ÅT = 223 K
c = 19.1304 (8) Å0.52 × 0.36 × 0.26 mm
Data collection top
Bruker SMART area-detector
diffractometer
6155 independent reflections
Absorption correction: multi-scan
(SADABS, Bruker, 2000)
4886 reflections with I > 2σ(I)
Tmin = 0.565, Tmax = 0.792Rint = 0.049
39717 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0570 restraints
wR(F2) = 0.137H-atom parameters constrained
S = 1.10Δρmax = 0.92 e Å3
6155 reflectionsΔρmin = 0.23 e Å3
253 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*/UeqOcc. (<1)
Zn0.50000.48584 (3)0.75000.03079 (11)
S10.36497 (4)0.46900 (5)0.74253 (3)0.03848 (15)
S20.48669 (4)0.33984 (6)0.64643 (4)0.04344 (17)
P10.38187 (4)0.36064 (5)0.66535 (3)0.03481 (15)
O20.33669 (12)0.39099 (14)0.59734 (9)0.0494 (5)
N10.50840 (11)0.61737 (16)0.67173 (10)0.0318 (4)
N20.49444 (12)0.96364 (18)0.52840 (12)0.0424 (5)
C10.36590 (15)0.1762 (2)0.73787 (13)0.0403 (6)
H10.41420.20610.75130.048*
C20.3811 (3)0.0635 (3)0.71081 (16)0.0794 (13)
H2A0.42160.06680.67740.095*
H2B0.33800.03540.68610.095*
C30.4007 (3)0.0156 (3)0.7705 (2)0.0846 (14)
H3A0.40960.08990.75140.102*
H3B0.44580.00990.79290.102*
C40.34220 (19)0.0219 (2)0.82339 (17)0.0552 (8)0.50
H4A0.35170.08070.85760.066*0.50
H4B0.29450.03430.80170.066*0.50
C50.3472 (7)0.0960 (9)0.8574 (5)0.081 (4)0.50
H5A0.31500.10070.89830.097*0.50
H5B0.39730.11140.87250.097*0.50
C60.3231 (7)0.1805 (10)0.8009 (6)0.078 (4)0.50
H6A0.32630.25560.82040.093*0.50
H6B0.27190.16650.78900.093*0.50
O10.34203 (10)0.24598 (14)0.68023 (9)0.0419 (4)0.50
C4'0.34220 (19)0.0219 (2)0.82339 (17)0.0552 (8)0.50
H4'10.36210.05580.86590.066*0.50
H4'20.30370.07100.80580.066*0.50
C5'0.3091 (5)0.0863 (10)0.8421 (5)0.060 (2)0.50
H5'10.34140.12360.87550.072*0.50
H5'20.26280.07200.86600.072*0.50
C6'0.2948 (5)0.1645 (9)0.7827 (6)0.047 (2)0.50
H6'10.28030.23730.80090.057*0.50
H6'20.25500.13590.75360.057*0.50
O1'0.34203 (10)0.24598 (14)0.68023 (9)0.0419 (4)0.50
C70.31081 (14)0.50087 (19)0.57852 (12)0.0368 (5)
H70.30100.54390.62160.044*
C80.24043 (17)0.4848 (3)0.53899 (16)0.0518 (7)
H8A0.24880.43480.49930.062*
H8B0.20420.45030.56970.062*
C90.21125 (17)0.5954 (3)0.51241 (16)0.0589 (8)
H9A0.19710.64150.55240.071*
H9B0.16750.58200.48410.071*
C100.26649 (18)0.6567 (2)0.46922 (16)0.0571 (8)
H10A0.24680.72940.45590.069*
H10B0.27640.61490.42630.069*
C110.3371 (2)0.6725 (3)0.50988 (18)0.0626 (9)
H11A0.32820.72100.55010.075*
H11B0.37340.70850.47990.075*
C120.36655 (15)0.5611 (2)0.53515 (16)0.0486 (6)
H12A0.37980.51540.49470.058*
H12B0.41060.57340.56310.058*
C130.55511 (13)0.61015 (19)0.61883 (12)0.0355 (5)
H130.58680.54880.61710.043*
C140.55932 (14)0.68874 (19)0.56618 (13)0.0371 (5)
H140.59210.67950.52890.045*
C150.51456 (13)0.78096 (19)0.56927 (12)0.0332 (5)
C160.46576 (14)0.78913 (18)0.62449 (12)0.0349 (5)
H160.43460.85080.62830.042*
C170.46358 (14)0.70568 (18)0.67361 (12)0.0342 (5)
H170.42930.71070.71000.041*
C180.51922 (14)0.8674 (2)0.51543 (13)0.0354 (5)
H180.54030.85160.47180.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.0474 (2)0.02128 (18)0.02365 (18)0.0000.00074 (15)0.000
S10.0513 (4)0.0333 (3)0.0309 (3)0.0008 (3)0.0006 (2)0.0033 (2)
S20.0554 (4)0.0307 (3)0.0441 (4)0.0004 (3)0.0075 (3)0.0010 (3)
P10.0529 (4)0.0230 (3)0.0285 (3)0.0013 (2)0.0050 (3)0.0021 (2)
O20.0852 (14)0.0275 (9)0.0356 (9)0.0066 (9)0.0194 (9)0.0011 (7)
N10.0499 (11)0.0222 (9)0.0232 (8)0.0018 (8)0.0023 (8)0.0021 (7)
N20.0629 (14)0.0280 (11)0.0363 (11)0.0016 (9)0.0044 (10)0.0124 (9)
C10.0527 (15)0.0342 (13)0.0339 (12)0.0116 (11)0.0034 (10)0.0077 (10)
C20.153 (4)0.0448 (18)0.0405 (16)0.035 (2)0.029 (2)0.0138 (14)
C30.121 (3)0.067 (2)0.065 (2)0.047 (2)0.040 (2)0.0328 (19)
C40.070 (2)0.0384 (15)0.0569 (18)0.0004 (13)0.0131 (15)0.0173 (13)
C50.175 (12)0.041 (4)0.026 (3)0.002 (7)0.019 (6)0.006 (3)
C60.135 (12)0.034 (4)0.064 (7)0.007 (6)0.043 (7)0.006 (4)
O10.0560 (11)0.0281 (9)0.0417 (9)0.0068 (8)0.0099 (8)0.0062 (7)
C4'0.070 (2)0.0384 (15)0.0569 (18)0.0004 (13)0.0131 (15)0.0173 (13)
C5'0.080 (6)0.060 (5)0.041 (5)0.001 (4)0.018 (4)0.010 (4)
C6'0.052 (4)0.032 (4)0.057 (6)0.000 (3)0.015 (3)0.005 (3)
O1'0.0560 (11)0.0281 (9)0.0417 (9)0.0068 (8)0.0099 (8)0.0062 (7)
C70.0546 (14)0.0262 (11)0.0296 (11)0.0069 (10)0.0070 (10)0.0024 (9)
C80.0555 (17)0.0512 (17)0.0485 (15)0.0079 (13)0.0087 (13)0.0058 (13)
C90.0550 (17)0.068 (2)0.0537 (17)0.0172 (15)0.0144 (14)0.0047 (16)
C100.079 (2)0.0377 (15)0.0547 (16)0.0071 (14)0.0267 (16)0.0078 (13)
C110.079 (2)0.0415 (16)0.068 (2)0.0104 (15)0.0286 (17)0.0169 (15)
C120.0499 (15)0.0439 (15)0.0519 (16)0.0009 (12)0.0092 (12)0.0051 (13)
C130.0505 (14)0.0253 (11)0.0307 (11)0.0057 (9)0.0063 (10)0.0038 (9)
C140.0508 (14)0.0284 (12)0.0322 (11)0.0024 (10)0.0078 (10)0.0060 (9)
C150.0473 (13)0.0220 (10)0.0303 (11)0.0023 (9)0.0017 (9)0.0056 (9)
C160.0495 (14)0.0210 (10)0.0343 (11)0.0051 (9)0.0009 (10)0.0024 (9)
C170.0520 (14)0.0230 (10)0.0277 (10)0.0042 (9)0.0058 (10)0.0017 (8)
C180.0457 (13)0.0285 (11)0.0319 (11)0.0027 (9)0.0003 (9)0.0084 (9)
Geometric parameters (Å, º) top
Zn—S12.4880 (7)C4'—H4'20.9800
Zn—S22.6600 (7)C5'—C6'1.498 (16)
Zn—N12.1850 (18)C5'—H5'10.9800
P1—S11.9946 (9)C5'—H5'20.9800
P1—S21.9716 (10)C6'—H6'10.9800
P1—O11.5876 (18)C6'—H6'20.9800
P1—O21.5849 (18)C7—C81.508 (4)
O2—C71.451 (3)C7—C121.503 (4)
N1—C131.328 (3)C7—H70.9900
N1—C171.344 (3)C8—C91.522 (4)
N2—N2i1.410 (4)C8—H8A0.9800
N2—C181.270 (3)C8—H8B0.9800
C1—C61.439 (13)C9—C101.501 (5)
C1—O1'1.454 (3)C9—H9A0.9800
C1—O11.454 (3)C9—H9B0.9800
C1—C21.478 (4)C10—C111.523 (4)
C1—C6'1.566 (11)C10—H10A0.9800
C1—H10.9900C10—H10B0.9800
C2—C31.530 (4)C11—C121.524 (4)
C2—H2A0.9800C11—H11A0.9800
C2—H2B0.9800C11—H11B0.9800
C3—C41.477 (5)C12—H12A0.9800
C3—H3A0.9800C12—H12B0.9800
C3—H3B0.9800C13—C141.384 (3)
C4—C51.565 (11)C13—H130.9400
C4—H4A0.9800C14—C151.382 (3)
C4—H4B0.9800C14—H140.9400
C5—C61.549 (16)C15—C161.388 (3)
C5—H5A0.9800C15—C181.467 (3)
C5—H5B0.9800C16—C171.376 (3)
C6—H6A0.9800C16—H160.9400
C6—H6B0.9800C17—H170.9400
C4'—C5'1.481 (12)C18—H180.9400
C4'—H4'10.9800
S1—Zn—S279.17 (2)C5'—C4'—H4'1108.6
S1—Zn—N195.15 (5)C3—C4'—H4'1108.6
S1—Zn—S1ii170.66 (3)C5'—C4'—H4'2108.6
S1—Zn—S2ii94.60 (2)C3—C4'—H4'2108.6
S1—Zn—N1ii91.62 (5)H4'1—C4'—H4'2107.6
S2—Zn—N188.57 (5)C4'—C5'—C6'116.2 (8)
S2—Zn—S2ii97.27 (3)C4'—C5'—H5'1108.2
S2—Zn—N1ii169.43 (5)C6'—C5'—H5'1108.2
N1ii—Zn—N187.09 (10)C4'—C5'—H5'2108.2
Zn—S1—P186.63 (3)C6'—C5'—H5'2108.2
Zn—S2—P182.46 (3)H5'1—C5'—H5'2107.4
S1—P1—S2111.74 (4)C5'—C6'—C1109.0 (8)
Zn—N1—C13121.33 (15)C5'—C6'—H6'1109.9
Zn—N1—C17120.79 (15)C1—C6'—H6'1109.9
C13—N1—C17117.79 (19)C5'—C6'—H6'2109.9
C18—N2—N2i111.4 (3)C1—C6'—H6'2109.9
O2—P1—O1'96.16 (10)H6'1—C6'—H6'2108.3
O2—P1—O196.16 (10)C1—O1'—P1120.02 (15)
O2—P1—S2112.83 (9)O2—C7—C8106.7 (2)
O1'—P1—S2111.77 (8)O2—C7—C12110.8 (2)
O1—P1—S2111.77 (8)C8—C7—C12111.5 (2)
O2—P1—S1112.06 (8)O2—C7—H7109.3
O1'—P1—S1111.38 (8)C8—C7—H7109.3
O1—P1—S1111.38 (8)C12—C7—H7109.3
C7—O2—P1125.79 (15)C7—C8—C9110.9 (2)
C6—C1—O1'116.7 (6)C7—C8—H8A109.5
C6—C1—O1116.7 (6)C9—C8—H8A109.5
C6—C1—C2115.4 (5)C7—C8—H8B109.5
O1'—C1—C2108.8 (2)C9—C8—H8B109.5
O1—C1—C2108.8 (2)H8A—C8—H8B108.1
O1'—C1—C6'102.5 (5)C8—C9—C10112.1 (3)
O1—C1—C6'102.5 (5)C8—C9—H9A109.2
C2—C1—C6'105.4 (5)C10—C9—H9A109.2
C6—C1—H1104.9C8—C9—H9B109.2
O1'—C1—H1104.9C10—C9—H9B109.2
O1—C1—H1104.9H9A—C9—H9B107.9
C2—C1—H1104.9C11—C10—C9110.7 (2)
C6'—C1—H1129.3C11—C10—H10A109.5
C1—C2—C3110.7 (3)C9—C10—H10A109.5
C1—C2—H2A109.5C11—C10—H10B109.5
C3—C2—H2A109.5C9—C10—H10B109.5
C1—C2—H2B109.5H10A—C10—H10B108.1
C3—C2—H2B109.5C12—C11—C10110.7 (2)
H2A—C2—H2B108.1C12—C11—H11A109.5
C4'—C3—C2111.9 (3)C10—C11—H11A109.5
C4—C3—C2111.9 (3)C12—C11—H11B109.5
C4'—C3—H3A109.2C10—C11—H11B109.5
C4—C3—H3A109.2H11A—C11—H11B108.1
C2—C3—H3A109.2C7—C12—C11111.0 (3)
C4'—C3—H3B109.2C7—C12—H12A109.4
C4—C3—H3B109.2C11—C12—H12A109.4
C2—C3—H3B109.2C7—C12—H12B109.4
H3A—C3—H3B107.9C11—C12—H12B109.4
C3—C4—C5101.3 (5)H12A—C12—H12B108.0
C3—C4—H4A111.5N1—C13—C14123.1 (2)
C5—C4—H4A111.5N1—C13—H13118.5
C3—C4—H4B111.5C14—C13—H13118.5
C5—C4—H4B111.5C13—C14—C15119.0 (2)
H4A—C4—H4B109.3C13—C14—H14120.5
C6—C5—C4106.8 (7)C15—C14—H14120.5
C6—C5—H5A110.4C14—C15—C16118.2 (2)
C4—C5—H5A110.4C14—C15—C18120.4 (2)
C6—C5—H5B110.4C16—C15—C18121.5 (2)
C4—C5—H5B110.4C17—C16—C15119.1 (2)
H5A—C5—H5B108.6C17—C16—H16120.4
C1—C6—C5114.0 (9)C15—C16—H16120.4
C1—C6—H6A108.8N1—C17—C16122.8 (2)
C5—C6—H6A108.8N1—C17—H17118.6
C1—C6—H6B108.8C16—C17—H17118.6
C5—C6—H6B108.8N2—C18—C15119.3 (2)
H6A—C6—H6B107.7N2—C18—H18120.3
C1—O1—P1120.02 (15)C15—C18—H18120.3
C5'—C4'—C3114.7 (5)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y, z+3/2.

Experimental details

Crystal data
Chemical formula[Zn(C12H22O2PS2)2(C12H10N4)]
Mr862.38
Crystal system, space groupOrthorhombic, Pbcn
Temperature (K)223
a, b, c (Å)18.3340 (8), 12.0404 (5), 19.1304 (8)
V3)4223.0 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.90
Crystal size (mm)0.52 × 0.36 × 0.26
Data collection
DiffractometerBruker SMART area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS, Bruker, 2000)
Tmin, Tmax0.565, 0.792
No. of measured, independent and
observed [I > 2σ(I)] reflections
39717, 6155, 4886
Rint0.049
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.057, 0.137, 1.10
No. of reflections6155
No. of parameters253
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.92, 0.23

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXTL (Bruker, 2000), PATTY in DIRDIF92 (Beurskens et al., 1992), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Zn—S12.4880 (7)P1—O21.5849 (18)
Zn—S22.6600 (7)N1—C131.328 (3)
Zn—N12.1850 (18)N1—C171.344 (3)
P1—S11.9946 (9)N2—N2i1.410 (4)
P1—S21.9716 (10)N2—C181.270 (3)
P1—O11.5876 (18)
S1—Zn—S279.17 (2)N1ii—Zn—N187.09 (10)
S1—Zn—N195.15 (5)Zn—S1—P186.63 (3)
S1—Zn—S1ii170.66 (3)Zn—S2—P182.46 (3)
S1—Zn—S2ii94.60 (2)S1—P1—S2111.74 (4)
S1—Zn—N1ii91.62 (5)Zn—N1—C13121.33 (15)
S2—Zn—N188.57 (5)Zn—N1—C17120.79 (15)
S2—Zn—S2ii97.27 (3)C13—N1—C17117.79 (19)
S2—Zn—N1ii169.43 (5)C18—N2—N2i111.4 (3)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y, z+3/2.
 

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