research communications
N-cyanodithioiminocarbonate)zinc
of dichloridobis(dimethylaLaboratoire de Chimie Minérale et Analytique, Département de Chimie, Faculté des Sciences et Techniques, Université Cheikh Anta Diop, Dakar, Senegal, and bDepartment of Chemistry and Biochemistry, University of Notre Dame, 246, Nieuwland, Science Hall, Notre Dame, IN 46557-5670, USA
*Correspondence e-mail: mouhamadoubdiop@gmail.com
The ZnII atom in the title complex, [ZnCl2(C4H6N2S2)2], is coordinated in a distorted tetrahedral manner by two Cl atoms and two terminal N atoms of two dimethyl N-cyanodithioiminocarbonate ligands. In the crystal, the complex molecules are connected through C—H⋯Cl hydrogen bonds and Cl⋯S contacts, leading to a two-dimensional structure extending parallel to the ab plane.
Keywords: crystal structure; zinc chloride adduct; dimethyl N-cyanodithioiminocarbonate; tetrahedral environment; layered structure.
CCDC reference: 1453191
1. Chemical context
Two N and two S atoms in dimethyl N-cyanodithioiminocarbonate (DMCDIC), which are expected to act as hard and soft donors, respectively, according to Pearson's concept, give an interesting coordination potential to this molecule. However, only one structure of a metal complex with DMCDIC acting as a ligand has been reported (Kojić-Prodić et al., 1992). Very recently, we reported the of [CoCl2(DMCDIC)2] (Diop et al., 2016). Because of the scarcity of data on the coordination ability of DMCDIC, we have focused on studying the interactions between some transition metal halides and this ligand, which has yielded the title complex.
2. Structural commentary
The structure of the title compound (Fig. 1) is isotypic with the Co complex reported recently (Diop et al., 2016). The ZnII atom is coordinated in a tetrahedral fashion by two Cl atoms and the cyanide N atoms of two dimethyl N-cyanodithioiminocarbonate ligands. The Zn atom has a τ4 value of 0.94 (Yang et al., 2007), indicating a near ideal tetrahedral geometry (τ4 = 1 for ideal tetrahedral and 0 for planar environments); τ4 = [360 - (α + β)]/141, where α and β are the two largest tetrahedral angles.
3. Supramolecular features
In the crystal, weak C—H⋯Cl hydrogen bonds (C3—H3B⋯Cl1ii and C7—H7B⋯Cl1ii; Table 1) link the molecules into inversion dimers (Fig. 2). The dimers are connected through a C4—H4B⋯Cl2i hydrogen bond (Table 1) and an S2⋯Cl2i short contact [3.3812 (7) Å], giving infinite chains along [10]. These chains are then connected through a longer hydrogen bond (C7—H7A⋯Cl2ii) and an S4⋯Cl2iv contact [3.3765 (7) Å; symmetry code: (iv) x, y, z + 1], leading to a layer parallel to the ab plane (Fig. 3).
4. Synthesis and crystallization
All chemicals are purchased from Aldrich Company, Germany and used as received. Dimethyl cyanocarbonimidodithioate was mixed in acetonitrile with ZnCl2 in a 1:1 ratio. Colourless block-like single crystals suitable for X-ray diffraction were obtained after a slow solvent evaporation at room temperature (303 K).
5. Refinement
Crystal data, data collection and structure . The structure was solved by incorporating the coordinates from the isotypic compound [Co((MeS)2CNCN)2Cl2] (Diop et al., 2016). Methyl H atoms were modeled as riding, with C—H = 0.98 Å and with Uiso(H) = 1.5Ueq(C), and were allowed to rotate to minimize their contribution to the electron density.
details are summarized in Table 2Supporting information
CCDC reference: 1453191
10.1107/S2056989016002607/is5443sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S2056989016002607/is5443Isup2.hkl
Two N and two S atoms in dimethyl N-cyanodithioiminocarbonate (DMCDIC), which are expected to act as hard and soft donors, respectively, according to Pearson's concept, gives an interesting coordination potential to this molecule. However, only one structure of metal complex with DMCDIC acting as a ligand has been reported (Kojić-Prodić et al., 1992). Very recently, we reported the
of [CoCl2(DMCDIC)2] (Diop et al., 2016). Because of the scarcity of data on the coordination ability of DMCDIC, we have focused on studying the interactions between some transition metal halides and this ligand, which has yielded the title complex.The structure of the title compound (Fig. 1) is isotypic with the Co complex reported recently (Diop et al., 2016). The Zn atom is coordinated in a tetrahedral fashion by two Cl atoms and the cyanide N atoms of two dimethyl N-cyanodithioiminocarbonate ligands. The Zn atom has a τ4 value of 0.94 (Yang et al., 2007), indicating a near ideal tetrahedral geometry (τ4 = 1 for ideal tetrahedral and 0 for planar environments); τ4 = [360 - (α + β)]/141, where α and β are the two largest tetrahedral angles.
In the crystal, weak C—H···Cl hydrogen bonds (C3—H3B···Cl1ii and C7—H7B···Cl1ii; Table 1) link the molecules into inversion dimers (Fig. 2). The dimers are connected through a C4—H4B···Cl2i hydrogen bond (Table 1) and an S2···Cl2i short contact [3.3812 (7) Å], giving infinite chains along [110]. These chains are then connected through a longer hydrogen bond (C7—H7A···Cl2ii) and an S4···Cl2iv contact [3.3765 (7) Å; symmetry code: (iv) x, y, z + 1], leading to a layer parallel to the ab plane (Fig. 3).
All chemicals are purchased from Aldrich Company, Germany and used as received. Dimethyl cyanocarbonimidodithioate was mixed in acetonitrile with ZnCl2 in a 1:1 ratio. Colourless block-like single crystals suitable for X-ray diffraction were obtained after a slow solvent evaporation at room temperature (303 K).
Crystal data, data collection and structure
details are summarized in Table 2. The structure was solved by incorporating the coordinates from the isotypic compound [Co((MeS)2CNCN)2Cl2] (Diop et al., 2016). Methyl H atoms were modeled as riding, with C—H = 0.98 Å and with Uiso(H) = 1.5Ueq(C), and were allowed to rotate to minimize their contribution to the electron density.Two N and two S atoms in dimethyl N-cyanodithioiminocarbonate (DMCDIC), which are expected to act as hard and soft donors, respectively, according to Pearson's concept, gives an interesting coordination potential to this molecule. However, only one structure of metal complex with DMCDIC acting as a ligand has been reported (Kojić-Prodić et al., 1992). Very recently, we reported the
of [CoCl2(DMCDIC)2] (Diop et al., 2016). Because of the scarcity of data on the coordination ability of DMCDIC, we have focused on studying the interactions between some transition metal halides and this ligand, which has yielded the title complex.The structure of the title compound (Fig. 1) is isotypic with the Co complex reported recently (Diop et al., 2016). The Zn atom is coordinated in a tetrahedral fashion by two Cl atoms and the cyanide N atoms of two dimethyl N-cyanodithioiminocarbonate ligands. The Zn atom has a τ4 value of 0.94 (Yang et al., 2007), indicating a near ideal tetrahedral geometry (τ4 = 1 for ideal tetrahedral and 0 for planar environments); τ4 = [360 - (α + β)]/141, where α and β are the two largest tetrahedral angles.
In the crystal, weak C—H···Cl hydrogen bonds (C3—H3B···Cl1ii and C7—H7B···Cl1ii; Table 1) link the molecules into inversion dimers (Fig. 2). The dimers are connected through a C4—H4B···Cl2i hydrogen bond (Table 1) and an S2···Cl2i short contact [3.3812 (7) Å], giving infinite chains along [110]. These chains are then connected through a longer hydrogen bond (C7—H7A···Cl2ii) and an S4···Cl2iv contact [3.3765 (7) Å; symmetry code: (iv) x, y, z + 1], leading to a layer parallel to the ab plane (Fig. 3).
All chemicals are purchased from Aldrich Company, Germany and used as received. Dimethyl cyanocarbonimidodithioate was mixed in acetonitrile with ZnCl2 in a 1:1 ratio. Colourless block-like single crystals suitable for X-ray diffraction were obtained after a slow solvent evaporation at room temperature (303 K).
detailsCrystal data, data collection and structure
details are summarized in Table 2. The structure was solved by incorporating the coordinates from the isotypic compound [Co((MeS)2CNCN)2Cl2] (Diop et al., 2016). Methyl H atoms were modeled as riding, with C—H = 0.98 Å and with Uiso(H) = 1.5Ueq(C), and were allowed to rotate to minimize their contribution to the electron density.Data collection: APEX2 (Bruker, 2015); cell
SAINT (Bruker, 2015); data reduction: SAINT (Bruker, 2015); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: Mercury (Macrae et al., 2006).Fig. 1. The molecular structure of the title compound. Atomic displacement ellipsoids are depicted at the 50% probability level and H atoms as spheres of an arbitrary radius. | |
Fig. 2. Packing diagram of the title compound, viewed approximately along the c axis, showing a pair of molecules. Displacement ellipsoids are as in Fig. 1. | |
Fig. 3. Packing diagram of the title compound viewed approximately along the c axis. Displacement ellipsoids are as in Fig. 1. |
[Zn(C4H6N2S2)2Cl2] | Z = 2 |
Mr = 428.73 | F(000) = 432 |
Triclinic, P1 | Dx = 1.709 Mg m−3 |
a = 8.8574 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 8.8833 (6) Å | Cell parameters from 8988 reflections |
c = 11.2391 (7) Å | θ = 2.3–28.6° |
α = 73.0839 (16)° | µ = 2.29 mm−1 |
β = 87.4301 (16)° | T = 120 K |
γ = 79.9801 (16)° | Block, colourless |
V = 833.14 (9) Å3 | 0.49 × 0.21 × 0.17 mm |
Bruker Kappa X8 APEXII diffractometer | 4239 independent reflections |
Radiation source: fine-focus sealed tube | 3939 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.6°, θmin = 1.9° |
combination of ω and φ–scans | h = −11→11 |
Absorption correction: numerical (SADABS; Krause et al., 2015) | k = −9→11 |
Tmin = 0.520, Tmax = 0.793 | l = −14→15 |
13605 measured reflections |
Refinement on F2 | Primary atom site location: isomorphous structure methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0275P)2 + 0.4996P] where P = (Fo2 + 2Fc2)/3 |
4239 reflections | (Δ/σ)max = 0.001 |
176 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
[Zn(C4H6N2S2)2Cl2] | γ = 79.9801 (16)° |
Mr = 428.73 | V = 833.14 (9) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.8574 (5) Å | Mo Kα radiation |
b = 8.8833 (6) Å | µ = 2.29 mm−1 |
c = 11.2391 (7) Å | T = 120 K |
α = 73.0839 (16)° | 0.49 × 0.21 × 0.17 mm |
β = 87.4301 (16)° |
Bruker Kappa X8 APEXII diffractometer | 4239 independent reflections |
Absorption correction: numerical (SADABS; Krause et al., 2015) | 3939 reflections with I > 2σ(I) |
Tmin = 0.520, Tmax = 0.793 | Rint = 0.019 |
13605 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 0 restraints |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.16 | Δρmax = 0.71 e Å−3 |
4239 reflections | Δρmin = −0.37 e Å−3 |
176 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. |
x | y | z | Uiso*/Ueq | ||
Zn1 | 0.31840 (2) | 0.80108 (2) | 0.23625 (2) | 0.01602 (6) | |
Cl1 | 0.16956 (5) | 0.61543 (5) | 0.29276 (4) | 0.02386 (9) | |
Cl2 | 0.23470 (5) | 1.01274 (5) | 0.08093 (4) | 0.02331 (9) | |
S1 | 0.83793 (5) | 0.41654 (5) | 0.37573 (4) | 0.01844 (9) | |
S2 | 0.97579 (4) | 0.27942 (5) | 0.17752 (4) | 0.01855 (9) | |
S3 | 0.53848 (5) | 0.72562 (5) | 0.68555 (4) | 0.01877 (9) | |
S4 | 0.35318 (5) | 0.94788 (5) | 0.80760 (4) | 0.01798 (9) | |
N1 | 0.52396 (16) | 0.69240 (17) | 0.19696 (14) | 0.0216 (3) | |
N2 | 0.73637 (16) | 0.50808 (17) | 0.14285 (13) | 0.0186 (3) | |
N3 | 0.34751 (18) | 0.87159 (18) | 0.38602 (13) | 0.0223 (3) | |
N4 | 0.31171 (17) | 0.95551 (17) | 0.57596 (13) | 0.0192 (3) | |
C1 | 0.62644 (18) | 0.60463 (19) | 0.17805 (15) | 0.0178 (3) | |
C2 | 0.83921 (17) | 0.41281 (18) | 0.22362 (15) | 0.0163 (3) | |
C3 | 1.0004 (2) | 0.2705 (2) | 0.44393 (16) | 0.0248 (3) | |
H3A | 0.9886 | 0.1666 | 0.4351 | 0.037* | |
H3B | 1.0075 | 0.2628 | 0.5323 | 0.037* | |
H3C | 1.0940 | 0.3023 | 0.4016 | 0.037* | |
C4 | 0.9182 (2) | 0.3114 (2) | 0.01991 (15) | 0.0230 (3) | |
H4A | 0.8123 | 0.2934 | 0.0184 | 0.034* | |
H4B | 0.9859 | 0.2369 | −0.0164 | 0.034* | |
H4C | 0.9249 | 0.4213 | −0.0285 | 0.034* | |
C5 | 0.33745 (19) | 0.90393 (19) | 0.47793 (15) | 0.0189 (3) | |
C6 | 0.39261 (18) | 0.88406 (19) | 0.67851 (15) | 0.0170 (3) | |
C7 | 0.6027 (2) | 0.6667 (2) | 0.84453 (16) | 0.0228 (3) | |
H7A | 0.6417 | 0.7550 | 0.8617 | 0.034* | |
H7B | 0.6845 | 0.5736 | 0.8586 | 0.034* | |
H7C | 0.5167 | 0.6393 | 0.9000 | 0.034* | |
C8 | 0.1918 (2) | 1.1031 (2) | 0.75497 (17) | 0.0237 (3) | |
H8A | 0.2209 | 1.1840 | 0.6817 | 0.036* | |
H8B | 0.1590 | 1.1526 | 0.8213 | 0.036* | |
H8C | 0.1075 | 1.0578 | 0.7330 | 0.036* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01630 (10) | 0.01660 (10) | 0.01569 (10) | 0.00008 (7) | 0.00063 (7) | −0.00723 (7) |
Cl1 | 0.02395 (19) | 0.0244 (2) | 0.0270 (2) | −0.00800 (15) | 0.00604 (15) | −0.01198 (16) |
Cl2 | 0.0288 (2) | 0.01982 (19) | 0.01917 (18) | 0.00453 (15) | −0.00438 (15) | −0.00668 (15) |
S1 | 0.01807 (18) | 0.02036 (19) | 0.01693 (18) | −0.00120 (14) | 0.00170 (14) | −0.00684 (14) |
S2 | 0.01730 (18) | 0.01884 (19) | 0.01817 (18) | 0.00245 (14) | 0.00138 (14) | −0.00662 (14) |
S3 | 0.02048 (18) | 0.01800 (19) | 0.01854 (19) | −0.00125 (14) | 0.00216 (14) | −0.00781 (14) |
S4 | 0.02055 (18) | 0.01868 (19) | 0.01489 (17) | 0.00057 (14) | −0.00022 (14) | −0.00732 (14) |
N1 | 0.0190 (7) | 0.0186 (7) | 0.0253 (7) | 0.0010 (5) | 0.0018 (5) | −0.0062 (6) |
N2 | 0.0176 (6) | 0.0185 (6) | 0.0183 (6) | 0.0011 (5) | 0.0019 (5) | −0.0058 (5) |
N3 | 0.0292 (7) | 0.0225 (7) | 0.0165 (7) | −0.0065 (6) | 0.0013 (5) | −0.0069 (5) |
N4 | 0.0243 (7) | 0.0190 (7) | 0.0150 (6) | −0.0034 (5) | 0.0006 (5) | −0.0063 (5) |
C1 | 0.0193 (7) | 0.0165 (7) | 0.0172 (7) | −0.0032 (6) | −0.0001 (6) | −0.0040 (6) |
C2 | 0.0151 (7) | 0.0153 (7) | 0.0186 (7) | −0.0032 (5) | 0.0031 (5) | −0.0052 (6) |
C3 | 0.0242 (8) | 0.0278 (9) | 0.0189 (8) | 0.0018 (7) | −0.0031 (6) | −0.0044 (7) |
C4 | 0.0245 (8) | 0.0267 (9) | 0.0174 (8) | 0.0016 (7) | 0.0007 (6) | −0.0094 (6) |
C5 | 0.0219 (8) | 0.0165 (7) | 0.0183 (7) | −0.0058 (6) | 0.0011 (6) | −0.0036 (6) |
C6 | 0.0193 (7) | 0.0162 (7) | 0.0168 (7) | −0.0052 (6) | 0.0027 (6) | −0.0060 (6) |
C7 | 0.0221 (8) | 0.0236 (8) | 0.0230 (8) | 0.0017 (6) | −0.0043 (6) | −0.0097 (7) |
C8 | 0.0256 (8) | 0.0212 (8) | 0.0229 (8) | 0.0049 (6) | −0.0024 (6) | −0.0090 (7) |
Zn1—N3 | 2.0003 (15) | N3—C5 | 1.146 (2) |
Zn1—N1 | 2.0016 (14) | N4—C5 | 1.308 (2) |
Zn1—Cl2 | 2.2030 (4) | N4—C6 | 1.317 (2) |
Zn1—Cl1 | 2.2210 (4) | C3—H3A | 0.9800 |
S1—C2 | 1.7191 (17) | C3—H3B | 0.9800 |
S1—C3 | 1.7922 (18) | C3—H3C | 0.9800 |
S2—C2 | 1.7141 (16) | C4—H4A | 0.9800 |
S2—C4 | 1.7935 (17) | C4—H4B | 0.9800 |
S3—C6 | 1.7228 (17) | C4—H4C | 0.9800 |
S3—C7 | 1.7980 (17) | C7—H7A | 0.9800 |
S4—C6 | 1.7067 (16) | C7—H7B | 0.9800 |
S4—C8 | 1.7914 (17) | C7—H7C | 0.9800 |
N1—C1 | 1.144 (2) | C8—H8A | 0.9800 |
N2—C1 | 1.309 (2) | C8—H8B | 0.9800 |
N2—C2 | 1.315 (2) | C8—H8C | 0.9800 |
N3—Zn1—N1 | 106.61 (6) | H3B—C3—H3C | 109.5 |
N3—Zn1—Cl2 | 108.82 (5) | S2—C4—H4A | 109.5 |
N1—Zn1—Cl2 | 110.62 (4) | S2—C4—H4B | 109.5 |
N3—Zn1—Cl1 | 107.09 (4) | H4A—C4—H4B | 109.5 |
N1—Zn1—Cl1 | 106.71 (4) | S2—C4—H4C | 109.5 |
Cl2—Zn1—Cl1 | 116.505 (19) | H4A—C4—H4C | 109.5 |
C2—S1—C3 | 103.78 (8) | H4B—C4—H4C | 109.5 |
C2—S2—C4 | 101.50 (8) | N3—C5—N4 | 172.64 (19) |
C6—S3—C7 | 103.40 (8) | N4—C6—S4 | 119.94 (13) |
C6—S4—C8 | 101.30 (8) | N4—C6—S3 | 121.19 (12) |
C1—N1—Zn1 | 166.17 (14) | S4—C6—S3 | 118.87 (9) |
C1—N2—C2 | 120.32 (15) | S3—C7—H7A | 109.5 |
C5—N3—Zn1 | 166.98 (14) | S3—C7—H7B | 109.5 |
C5—N4—C6 | 120.40 (15) | H7A—C7—H7B | 109.5 |
N1—C1—N2 | 172.98 (18) | S3—C7—H7C | 109.5 |
N2—C2—S2 | 119.54 (12) | H7A—C7—H7C | 109.5 |
N2—C2—S1 | 121.40 (12) | H7B—C7—H7C | 109.5 |
S2—C2—S1 | 119.05 (9) | S4—C8—H8A | 109.5 |
S1—C3—H3A | 109.5 | S4—C8—H8B | 109.5 |
S1—C3—H3B | 109.5 | H8A—C8—H8B | 109.5 |
H3A—C3—H3B | 109.5 | S4—C8—H8C | 109.5 |
S1—C3—H3C | 109.5 | H8A—C8—H8C | 109.5 |
H3A—C3—H3C | 109.5 | H8B—C8—H8C | 109.5 |
C1—N2—C2—S2 | 176.35 (12) | C5—N4—C6—S4 | −177.58 (12) |
C1—N2—C2—S1 | −2.5 (2) | C5—N4—C6—S3 | 2.2 (2) |
C4—S2—C2—N2 | −3.57 (15) | C8—S4—C6—N4 | 2.39 (15) |
C4—S2—C2—S1 | 175.32 (10) | C8—S4—C6—S3 | −177.42 (10) |
C3—S1—C2—N2 | −178.77 (14) | C7—S3—C6—N4 | −176.93 (14) |
C3—S1—C2—S2 | 2.36 (12) | C7—S3—C6—S4 | 2.89 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4B···Cl2i | 0.98 | 2.73 | 3.4486 (18) | 131 |
C3—H3B···Cl1ii | 0.98 | 2.80 | 3.5868 (19) | 137 |
C7—H7A···Cl2iii | 0.98 | 2.74 | 3.7165 (18) | 176 |
C7—H7B···Cl1ii | 0.98 | 2.84 | 3.5976 (18) | 134 |
Symmetry codes: (i) x+1, y−1, z; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4B···Cl2i | 0.98 | 2.73 | 3.4486 (18) | 131 |
C3—H3B···Cl1ii | 0.98 | 2.80 | 3.5868 (19) | 137 |
C7—H7A···Cl2iii | 0.98 | 2.74 | 3.7165 (18) | 176 |
C7—H7B···Cl1ii | 0.98 | 2.84 | 3.5976 (18) | 134 |
Symmetry codes: (i) x+1, y−1, z; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Zn(C4H6N2S2)2Cl2] |
Mr | 428.73 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 120 |
a, b, c (Å) | 8.8574 (5), 8.8833 (6), 11.2391 (7) |
α, β, γ (°) | 73.0839 (16), 87.4301 (16), 79.9801 (16) |
V (Å3) | 833.14 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.29 |
Crystal size (mm) | 0.49 × 0.21 × 0.17 |
Data collection | |
Diffractometer | Bruker Kappa X8 APEXII |
Absorption correction | Numerical (SADABS; Krause et al., 2015) |
Tmin, Tmax | 0.520, 0.793 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13605, 4239, 3939 |
Rint | 0.019 |
(sin θ/λ)max (Å−1) | 0.673 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.062, 1.16 |
No. of reflections | 4239 |
No. of parameters | 176 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.71, −0.37 |
Computer programs: APEX2 (Bruker, 2015), SAINT (Bruker, 2015), SHELXT2014 (Sheldrick, 2015a), SHELXL2014 (Sheldrick, 2015b), XP in SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2006).
Acknowledgements
The authors acknowledge Cheikh Anta Diop University of Dakar (Sénégal) and the University of Notre Dame (USA) for financial support.
References
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