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The title complex, [Ni(C5H8NOS2)Cl(C18H15P)], exhibits a four-coordinate Ni atom in a slightly distorted square-planar geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702209X/im2015sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680702209X/im2015Isup2.hkl
Contains datablock I

CCDC reference: 650620

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.027
  • wR factor = 0.079
  • Data-to-parameter ratio = 16.4

checkCIF/PLATON results

No syntax errors found




Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. crimson PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - S1 .. 6.38 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - S2 .. 6.92 su
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 0 ALERT type 5 Informative message, check

Comment top

Dithiocarbamates have been studied extensively over recent decades in response to their growing applications in many areas such as industry, biology and analytical chemistry. The N,N-disubstituted dithiocarbamate residue (dtc) is the classical bidentate ligand and one of the most frequently used sulfur donors (Cambridge Structural Database, 2007 with updates; Allen, 2002). Recently we began to devote our interest to Ni complexes where this ligand is simultaneously accompanied by a halogene and phosphine.

Here we describe a new product - (4-morpholinecarbodithioato-S,S')-chloro-(triphenylphosphine)-nickel(II)(I) (Scheme I) obtained by essentially quantitative metathesis of trans-dichloro-bis(triphenylphosphine)-nickel(II) (Garton et al., 1963) and bis(4-morpholinecarbodithioato-S,S') nickel(II) prepared in situ.

For our purposes we have chosen a dithiocarbamate ligand derived from a cyclic amine. Interestingly, only a few complexes of this kind have been structurally characterized. For Ni four such compounds may be quoted, among them two containing a chloro (Pastorek et al., 1999, Pavlicek et al., 2003) and two with a bromo ligand (Pastorek et al., 1996, Pavlicek et al., 2003). In addition, one Pd containing complex has recently been described (Shaheen et al., 2006).

The molecular structure of (I) with atom numbering scheme is shown in Fig.1. The single-crystal X-ray analysis proved, as expected, a distorted square-planar arrangement of the NiS2ClP complex core. The dtc ligand acts as a bidentate chelating ligand, coordinating to Ni via both S atoms. Atom S1 is located trans to the triphenylphosphine ligand and atom S2 is trans to the Cl ligand. The slight deformation of the coordination geometry is probably caused by the presence of both chelating agent and sterically hindered phosphine.

It is noteworthy that (I) which was recrystallized from chloroform as were all four aforementioned Ni complexes, does not retain the solvent within its crystal structure. It therefore resembles the Pd-containing complex, which was crystallized from dichloromethane and obviously does not contain chloroform.

A closer look at (I) reveals some short contacts CmorphH···Cl, within a pair of molecules (Fig. 2), which may suggest that some additional weak interractions are present. This corresponds to the slightly longer Ni—Cl bond length and smaller P—Ni—Cl angle comparing to the previously mentioned species.

Related literature top

For related literature, see: Allen (2002); Garton et al. (1963); Pastorek et al. (1996, 1999); Pavlicek et al. (2003); Shaheen et al. (2006).

Experimental top

Nickel chloride, NiCl2 × 6H2O (0.608 g, 0.0025 mol, purchased from POCh) was dissolved in 50 ml of methanol/water (10/1, v/v) and this solution was added dropwise to the potassium salt of 4-morpholinecarbodithioic acid OC4H8NCS2K (1.03 g, 0.005 mol) dissolved in methanol/water. The mixture was stirred vigorously in an inert gas (Ar) atmosphere for 30 minutes, then filtered and left for crystallization at 5° C. After ca. two weeks green crystalline product, namely Ni(S2CNC4H8O)2 was collected. It was again dissolved (0.206 g, 0.00058 mol) in 10 ml of chloroform and mixed with solution of equimolar amount of NiCl2(PPh3)2 (0.379 g). The mixture which turned to deep violet, was stirred for 10 minutes and then filtered. To the solution 10 ml of Et2O was added. After15 minutes crimson-violet crystals were collected and washed with several portions of ether.

Refinement top

All H atoms were placed in calculated positions (0.95 Å for CH aryl and 0.99 Å for CH2 alkyl) and refined as riding with Uiso(H) = 1.2Ueq (aryl carrier) or 1.3Ueq (methylene carrier).

Structure description top

Dithiocarbamates have been studied extensively over recent decades in response to their growing applications in many areas such as industry, biology and analytical chemistry. The N,N-disubstituted dithiocarbamate residue (dtc) is the classical bidentate ligand and one of the most frequently used sulfur donors (Cambridge Structural Database, 2007 with updates; Allen, 2002). Recently we began to devote our interest to Ni complexes where this ligand is simultaneously accompanied by a halogene and phosphine.

Here we describe a new product - (4-morpholinecarbodithioato-S,S')-chloro-(triphenylphosphine)-nickel(II)(I) (Scheme I) obtained by essentially quantitative metathesis of trans-dichloro-bis(triphenylphosphine)-nickel(II) (Garton et al., 1963) and bis(4-morpholinecarbodithioato-S,S') nickel(II) prepared in situ.

For our purposes we have chosen a dithiocarbamate ligand derived from a cyclic amine. Interestingly, only a few complexes of this kind have been structurally characterized. For Ni four such compounds may be quoted, among them two containing a chloro (Pastorek et al., 1999, Pavlicek et al., 2003) and two with a bromo ligand (Pastorek et al., 1996, Pavlicek et al., 2003). In addition, one Pd containing complex has recently been described (Shaheen et al., 2006).

The molecular structure of (I) with atom numbering scheme is shown in Fig.1. The single-crystal X-ray analysis proved, as expected, a distorted square-planar arrangement of the NiS2ClP complex core. The dtc ligand acts as a bidentate chelating ligand, coordinating to Ni via both S atoms. Atom S1 is located trans to the triphenylphosphine ligand and atom S2 is trans to the Cl ligand. The slight deformation of the coordination geometry is probably caused by the presence of both chelating agent and sterically hindered phosphine.

It is noteworthy that (I) which was recrystallized from chloroform as were all four aforementioned Ni complexes, does not retain the solvent within its crystal structure. It therefore resembles the Pd-containing complex, which was crystallized from dichloromethane and obviously does not contain chloroform.

A closer look at (I) reveals some short contacts CmorphH···Cl, within a pair of molecules (Fig. 2), which may suggest that some additional weak interractions are present. This corresponds to the slightly longer Ni—Cl bond length and smaller P—Ni—Cl angle comparing to the previously mentioned species.

For related literature, see: Allen (2002); Garton et al. (1963); Pastorek et al. (1996, 1999); Pavlicek et al. (2003); Shaheen et al. (2006).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al., 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. Molecular structure and atom-numbering scheme for I with displacement ellipsoids drawn at the 50% probability level.
[Figure 2] Fig. 2. Schematic drawing of the crystal packing of I showing short contacts within a pair of molecules. (C4···Cl1' 3.581 Å, C5···Cl1' 3.432 Å)
Chlorido(4-morpholinecarbodithioato- κ2S,S')(triphenylphosphine)nickel(II) top
Crystal data top
[Ni(C5H8NOS2)Cl(C18H15P)]Z = 2
Mr = 518.67F(000) = 536
Triclinic, P1Dx = 1.517 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.4814 (8) ÅCell parameters from 10672 reflections
b = 10.6009 (9) Åθ = 2.2–32.4°
c = 13.243 (1) ŵ = 1.24 mm1
α = 111.908 (8)°T = 120 K
β = 91.044 (7)°Prism, crimson-violet
γ = 110.924 (8)°0.24 × 0.16 × 0.06 mm
V = 1135.7 (2) Å3
Data collection top
4-axis κ geometry
diffractometer
4448 independent reflections
Graphite monochromator4283 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm-1Rint = 0.011
ω scans, 0.75° widthθmax = 26°, θmin = 2.2°
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2006); analytical numeric absorption correction using a multifaceted crystal model (Clark & Reid, 1995)]
h = 119
Tmin = 0.621, Tmax = 0.843k = 1313
8344 measured reflectionsl = 1316
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.13 w = 1/[σ2(Fo2) + (0.0476P)2 + 0.6214P]
where P = (Fo2 + 2Fc2)/3
4448 reflections(Δ/σ)max < 0.001
271 parametersΔρmax = 0.56 e Å3
0 restraintsΔρmin = 0.37 e Å3
Crystal data top
[Ni(C5H8NOS2)Cl(C18H15P)]γ = 110.924 (8)°
Mr = 518.67V = 1135.7 (2) Å3
Triclinic, P1Z = 2
a = 9.4814 (8) ÅMo Kα radiation
b = 10.6009 (9) ŵ = 1.24 mm1
c = 13.243 (1) ÅT = 120 K
α = 111.908 (8)°0.24 × 0.16 × 0.06 mm
β = 91.044 (7)°
Data collection top
4-axis κ geometry
diffractometer
4448 independent reflections
Absorption correction: analytical
[CrysAlis RED (Oxford Diffraction, 2006); analytical numeric absorption correction using a multifaceted crystal model (Clark & Reid, 1995)]
4283 reflections with I > 2σ(I)
Tmin = 0.621, Tmax = 0.843Rint = 0.011
8344 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 1.13Δρmax = 0.56 e Å3
4448 reflectionsΔρmin = 0.37 e Å3
271 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
Ni10.71797 (2)0.33190 (2)0.119811 (16)0.01561 (8)
Cl10.68831 (5)0.24822 (5)0.24958 (3)0.02355 (11)
S10.68647 (5)0.11482 (5)0.01212 (3)0.01960 (11)
S20.75229 (5)0.38803 (5)0.02326 (3)0.01922 (11)
P10.70778 (5)0.53984 (5)0.23183 (3)0.01527 (10)
O10.64896 (15)0.00309 (15)0.43865 (10)0.0268 (3)
N10.71309 (16)0.14260 (16)0.20607 (12)0.0206 (3)
C10.71688 (18)0.20381 (19)0.09929 (14)0.0178 (3)
C20.7558 (2)0.2294 (2)0.27353 (14)0.0236 (4)
H2A0.86290.2470.2850.031*
H2B0.74950.32650.23430.031*
C30.6494 (2)0.1474 (2)0.38444 (14)0.0246 (4)
H3A0.54420.13980.37340.032*
H3B0.68360.20310.43120.032*
C40.6860 (2)0.0152 (2)0.26313 (15)0.0239 (4)
H4A0.63460.06910.21830.031*
H4B0.78520.02570.27230.031*
C50.5861 (2)0.0805 (2)0.37556 (15)0.0275 (4)
H5A0.57640.18350.41640.036*
H5B0.48230.08250.36550.036*
C60.83379 (19)0.64355 (18)0.36638 (13)0.0174 (3)
C70.8329 (2)0.77928 (19)0.43852 (14)0.0215 (3)
H70.76310.81550.41880.026*
C80.9336 (2)0.8608 (2)0.53860 (15)0.0248 (4)
H80.93190.95230.58740.03*
C91.0368 (2)0.8096 (2)0.56801 (15)0.0254 (4)
H91.10560.86580.63660.03*
C101.0392 (2)0.6759 (2)0.49680 (15)0.0231 (4)
H101.10980.64070.51670.028*
C110.93838 (19)0.59321 (19)0.39625 (14)0.0195 (3)
H110.94080.50190.34770.023*
C120.51067 (19)0.49114 (18)0.25703 (14)0.0185 (3)
C130.4727 (2)0.5150 (2)0.36186 (15)0.0244 (4)
H130.55160.56640.4250.029*
C140.3195 (2)0.4639 (2)0.37452 (17)0.0300 (4)
H140.29450.48040.44620.036*
C150.2038 (2)0.3891 (2)0.28266 (17)0.0283 (4)
H150.09950.35350.29130.034*
C160.2406 (2)0.3662 (2)0.17825 (17)0.0297 (4)
H160.16130.31640.11540.036*
C170.3933 (2)0.4161 (2)0.16519 (15)0.0252 (4)
H170.41780.3990.09330.03*
C180.74246 (18)0.68505 (18)0.18132 (13)0.0164 (3)
C190.64409 (19)0.75773 (19)0.18590 (14)0.0203 (3)
H190.54910.72620.21020.024*
C200.6844 (2)0.8761 (2)0.15500 (16)0.0243 (4)
H200.61650.92450.15770.029*
C210.8233 (2)0.9237 (2)0.12022 (15)0.0242 (4)
H210.85211.00670.10170.029*
C220.9203 (2)0.8495 (2)0.11252 (15)0.0225 (4)
H221.01420.88030.08680.027*
C230.87987 (19)0.73035 (19)0.14237 (14)0.0188 (3)
H230.94590.67940.13630.023*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01970 (13)0.01613 (13)0.01347 (12)0.00895 (9)0.00388 (9)0.00673 (9)
Cl10.0342 (2)0.0194 (2)0.0179 (2)0.00850 (17)0.00356 (17)0.01034 (16)
S10.0269 (2)0.0181 (2)0.0159 (2)0.01110 (17)0.00499 (16)0.00700 (16)
S20.0254 (2)0.0184 (2)0.0147 (2)0.00875 (17)0.00347 (16)0.00747 (16)
P10.0180 (2)0.0169 (2)0.0138 (2)0.00887 (16)0.00428 (15)0.00719 (16)
O10.0284 (7)0.0323 (7)0.0155 (6)0.0111 (6)0.0052 (5)0.0059 (5)
N10.0200 (7)0.0219 (7)0.0187 (7)0.0068 (6)0.0041 (6)0.0084 (6)
C10.0146 (7)0.0203 (8)0.0190 (8)0.0070 (6)0.0019 (6)0.0083 (7)
C20.0231 (9)0.0272 (9)0.0168 (8)0.0047 (7)0.0026 (7)0.0100 (7)
C30.0241 (9)0.0315 (10)0.0161 (8)0.0101 (7)0.0033 (7)0.0082 (7)
C40.0273 (9)0.0235 (9)0.0177 (8)0.0108 (7)0.0045 (7)0.0042 (7)
C50.0291 (9)0.0266 (9)0.0191 (9)0.0084 (8)0.0034 (7)0.0036 (7)
C60.0200 (8)0.0192 (8)0.0145 (7)0.0072 (6)0.0048 (6)0.0088 (6)
C70.0257 (8)0.0220 (9)0.0195 (8)0.0115 (7)0.0067 (7)0.0091 (7)
C80.0305 (9)0.0208 (9)0.0195 (8)0.0081 (7)0.0084 (7)0.0062 (7)
C90.0242 (9)0.0268 (9)0.0171 (8)0.0011 (7)0.0009 (7)0.0092 (7)
C100.0211 (8)0.0277 (9)0.0233 (9)0.0076 (7)0.0025 (7)0.0154 (7)
C110.0211 (8)0.0201 (8)0.0192 (8)0.0077 (7)0.0053 (6)0.0104 (7)
C120.0195 (8)0.0183 (8)0.0212 (8)0.0089 (6)0.0064 (6)0.0100 (7)
C130.0245 (9)0.0329 (10)0.0206 (9)0.0139 (8)0.0055 (7)0.0132 (7)
C140.0297 (10)0.0449 (12)0.0282 (10)0.0203 (9)0.0150 (8)0.0224 (9)
C150.0216 (9)0.0340 (10)0.0397 (11)0.0135 (8)0.0115 (8)0.0230 (9)
C160.0218 (9)0.0333 (10)0.0302 (10)0.0070 (8)0.0015 (7)0.0127 (8)
C170.0244 (9)0.0295 (9)0.0196 (8)0.0095 (7)0.0047 (7)0.0087 (7)
C180.0187 (8)0.0168 (8)0.0139 (7)0.0080 (6)0.0016 (6)0.0055 (6)
C190.0192 (8)0.0212 (8)0.0221 (8)0.0094 (7)0.0039 (7)0.0089 (7)
C200.0239 (9)0.0224 (9)0.0300 (9)0.0127 (7)0.0004 (7)0.0109 (7)
C210.0249 (9)0.0212 (8)0.0270 (9)0.0060 (7)0.0012 (7)0.0134 (7)
C220.0185 (8)0.0255 (9)0.0224 (9)0.0055 (7)0.0015 (7)0.0116 (7)
C230.0178 (8)0.0217 (8)0.0183 (8)0.0091 (6)0.0022 (6)0.0085 (7)
Geometric parameters (Å, º) top
Ni1—S22.1852 (5)C8—H80.95
Ni1—P12.1877 (5)C9—C101.387 (3)
Ni1—Cl12.1900 (5)C9—H90.95
Ni1—S12.2197 (5)C10—C111.393 (2)
S1—C11.7136 (17)C10—H100.95
S2—C11.7298 (18)C11—H110.95
P1—C121.8256 (17)C12—C131.393 (2)
P1—C61.8258 (17)C12—C171.395 (3)
P1—C181.8275 (17)C13—C141.395 (3)
O1—C51.425 (2)C13—H130.95
O1—C31.426 (2)C14—C151.387 (3)
N1—C11.311 (2)C14—H140.95
N1—C21.473 (2)C15—C161.386 (3)
N1—C41.476 (2)C15—H150.95
C2—C31.516 (2)C16—C171.392 (3)
C2—H2A0.99C16—H160.95
C2—H2B0.99C17—H170.95
C3—H3A0.99C18—C191.396 (2)
C3—H3B0.99C18—C231.399 (2)
C4—C51.518 (3)C19—C201.391 (2)
C4—H4A0.99C19—H190.95
C4—H4B0.99C20—C211.386 (3)
C5—H5A0.99C20—H200.95
C5—H5B0.99C21—C221.391 (3)
C6—C111.395 (2)C21—H210.95
C6—C71.402 (2)C22—C231.389 (2)
C7—C81.387 (3)C22—H220.95
C7—H70.95C23—H230.95
C8—C91.389 (3)
S2—Ni1—P196.597 (18)C6—C7—H7119.9
S2—Ni1—Cl1172.162 (18)C7—C8—C9120.50 (17)
P1—Ni1—Cl191.198 (18)C7—C8—H8119.8
S2—Ni1—S178.878 (18)C9—C8—H8119.8
P1—Ni1—S1168.831 (19)C10—C9—C8119.73 (17)
Cl1—Ni1—S193.595 (18)C10—C9—H9120.1
C1—S1—Ni185.84 (6)C8—C9—H9120.1
C1—S2—Ni186.54 (6)C9—C10—C11120.21 (16)
C12—P1—C6107.31 (8)C9—C10—H10119.9
C12—P1—C18105.46 (7)C11—C10—H10119.9
C6—P1—C18101.02 (7)C10—C11—C6120.40 (16)
C12—P1—Ni1105.29 (6)C10—C11—H11119.8
C6—P1—Ni1119.15 (6)C6—C11—H11119.8
C18—P1—Ni1117.59 (5)C13—C12—C17119.06 (16)
C5—O1—C3109.06 (13)C13—C12—P1123.20 (14)
C1—N1—C2122.46 (15)C17—C12—P1117.55 (13)
C1—N1—C4121.45 (15)C12—C13—C14120.36 (18)
C2—N1—C4115.58 (14)C12—C13—H13119.8
N1—C1—S1125.79 (14)C14—C13—H13119.8
N1—C1—S2125.49 (13)C15—C14—C13120.13 (17)
S1—C1—S2108.72 (10)C15—C14—H14119.9
N1—C2—C3110.18 (14)C13—C14—H14119.9
N1—C2—H2A109.6C16—C15—C14119.83 (17)
C3—C2—H2A109.6C16—C15—H15120.1
N1—C2—H2B109.6C14—C15—H15120.1
C3—C2—H2B109.6C15—C16—C17120.21 (18)
H2A—C2—H2B108.1C15—C16—H16119.9
O1—C3—C2110.34 (15)C17—C16—H16119.9
O1—C3—H3A109.6C16—C17—C12120.40 (17)
C2—C3—H3A109.6C16—C17—H17119.8
O1—C3—H3B109.6C12—C17—H17119.8
C2—C3—H3B109.6C19—C18—C23119.05 (15)
H3A—C3—H3B108.1C19—C18—P1123.48 (13)
N1—C4—C5109.61 (15)C23—C18—P1117.36 (12)
N1—C4—H4A109.7C20—C19—C18120.33 (16)
C5—C4—H4A109.7C20—C19—H19119.8
N1—C4—H4B109.7C18—C19—H19119.8
C5—C4—H4B109.7C21—C20—C19120.26 (16)
H4A—C4—H4B108.2C21—C20—H20119.9
O1—C5—C4111.48 (15)C19—C20—H20119.9
O1—C5—H5A109.3C20—C21—C22119.84 (16)
C4—C5—H5A109.3C20—C21—H21120.1
O1—C5—H5B109.3C22—C21—H21120.1
C4—C5—H5B109.3C23—C22—C21120.07 (16)
H5A—C5—H5B108C23—C22—H22120
C11—C6—C7119.04 (16)C21—C22—H22120
C11—C6—P1120.51 (13)C22—C23—C18120.39 (15)
C7—C6—P1120.35 (13)C22—C23—H23119.8
C8—C7—C6120.13 (16)C18—C23—H23119.8
C8—C7—H7119.9

Experimental details

Crystal data
Chemical formula[Ni(C5H8NOS2)Cl(C18H15P)]
Mr518.67
Crystal system, space groupTriclinic, P1
Temperature (K)120
a, b, c (Å)9.4814 (8), 10.6009 (9), 13.243 (1)
α, β, γ (°)111.908 (8), 91.044 (7), 110.924 (8)
V3)1135.7 (2)
Z2
Radiation typeMo Kα
µ (mm1)1.24
Crystal size (mm)0.24 × 0.16 × 0.06
Data collection
Diffractometer4-axis κ geometry
Absorption correctionAnalytical
[CrysAlis RED (Oxford Diffraction, 2006); analytical numeric absorption correction using a multifaceted crystal model (Clark & Reid, 1995)]
Tmin, Tmax0.621, 0.843
No. of measured, independent and
observed [I > 2σ(I)] reflections
8344, 4448, 4283
Rint0.011
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.079, 1.13
No. of reflections4448
No. of parameters271
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.56, 0.37

Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), CrysAlis RED, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al., 2006), WinGX (Farrugia, 1999).

 

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