Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807040597/bh2125sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807040597/bh2125Isup2.hkl |
CCDC reference: 660148
Key indicators
- Single-crystal X-ray study
- T = 105 K
- Mean (C-C) = 0.006 Å
- R factor = 0.040
- wR factor = 0.112
- Data-to-parameter ratio = 19.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density .... 6.44 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C13
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C14
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 3 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 5 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
For the preparation of the diphosphine ligand, see: Klausmeyer et al. (2004).
The DPP ligand is an impurity formed in the synthesis of PCP-31 (Klausmeyer et al., 2004). Then combined with an equivalent of Ag(I)OTF in 10 ml CH3CN, a clear colorless solution results. Colorless blocks of the title compound were obtained by the slow diffusion of ether into a CH3CN solution containing the complex at 278 K.
H atoms were included in calculated positions and refined as riding on their parent atoms, with C—H bond lengths fixed to 0.95 (aromatic CH), or 0.98 Å (methyl CH3). Isotropic displacement parameters were fixed for H atoms: Uiso(H) = 1.5Ueq(C15) for the methyl group and Uiso(H) = 1.2Ueq(carrier C) for phenyl groups. In the last difference map, the highest residual peak, 1.47 e.Å-3, is found at 1.03 Å from Ag1.
The title polymer contains AgI ions in pseudo tetrahedral geometry bridged by a rigid bidentate diphosphine (DPP) ligand (Klausmeyer et al., 2004). The distorted tetrahedral angles range from 140.60 (10) to 86.61 (13)°. The AgI ion is stabilized by the soft donor phosphorus, from DPP, and 2 hard oxo ligands, from trifluoromethanesulfonate. The structure contains an 8-membered ring containing the silvers and the anions (Fig. 1). This ring is situated on an inversion center. The rings are then linked by the diphosphine ligand through the silvers into a one-dimensional polymer which boasts a 'Ring—P—P—Ring' design resembling a staircase (Fig. 2). The extended packing structure indicates that F atoms on the trifluoromethanesulfonate ion form a 3.186 (4) Å interaction with a C—H group on a neighboring 'staircase' polymer.
For the preparation of the diphosphine ligand, see: Klausmeyer et al. (2004).
Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2 (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2003); software used to prepare material for publication: SHELXTL (Bruker, 2003).
[Ag2(CF3SO3)2(C28H26N2P2)] | F(000) = 956 |
Mr = 483.16 | Dx = 1.771 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8448 reflections |
a = 10.1128 (2) Å | θ = 2.3–28.0° |
b = 17.4753 (3) Å | µ = 1.36 mm−1 |
c = 10.5053 (2) Å | T = 105 K |
β = 102.599 (1)° | Rod, colourless |
V = 1811.84 (6) Å3 | 0.21 × 0.17 × 0.10 mm |
Z = 4 |
Bruker X8 APEX diffractometer | 4502 independent reflections |
Radiation source: fine-focus sealed tube | 3588 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 28.3°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.760, Tmax = 0.873 | k = −23→23 |
28681 measured reflections | l = −14→12 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0619P)2 + 1.0373P] where P = (Fo2 + 2Fc2)/3 |
4502 reflections | (Δ/σ)max < 0.001 |
227 parameters | Δρmax = 1.47 e Å−3 |
0 restraints | Δρmin = −0.23 e Å−3 |
[Ag2(CF3SO3)2(C28H26N2P2)] | V = 1811.84 (6) Å3 |
Mr = 483.16 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.1128 (2) Å | µ = 1.36 mm−1 |
b = 17.4753 (3) Å | T = 105 K |
c = 10.5053 (2) Å | 0.21 × 0.17 × 0.10 mm |
β = 102.599 (1)° |
Bruker X8 APEX diffractometer | 4502 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3588 reflections with I > 2σ(I) |
Tmin = 0.760, Tmax = 0.873 | Rint = 0.030 |
28681 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.112 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.47 e Å−3 |
4502 reflections | Δρmin = −0.23 e Å−3 |
227 parameters |
x | y | z | Uiso*/Ueq | ||
Ag1 | 0.61713 (3) | 1.022971 (14) | 0.25471 (3) | 0.05425 (11) | |
P1 | 0.50042 (7) | 0.96768 (4) | 0.40910 (7) | 0.03942 (17) | |
S3 | 0.57444 (9) | 0.87763 (4) | 0.03092 (8) | 0.05077 (19) | |
C7 | 0.3200 (3) | 0.95576 (16) | 0.3394 (3) | 0.0439 (6) | |
C8 | 0.2762 (4) | 0.9755 (2) | 0.2101 (4) | 0.0623 (9) | |
H8 | 0.3393 | 0.9941 | 0.1624 | 0.075* | |
C1 | 0.5731 (3) | 0.87625 (16) | 0.4756 (3) | 0.0442 (6) | |
C2 | 0.6818 (4) | 0.8485 (2) | 0.4273 (4) | 0.0607 (8) | |
H2 | 0.7138 | 0.8765 | 0.3627 | 0.073* | |
C6 | 0.5306 (4) | 0.83521 (19) | 0.5713 (4) | 0.0590 (8) | |
H6 | 0.4571 | 0.8535 | 0.6057 | 0.071* | |
C4 | 0.6990 (4) | 0.7402 (2) | 0.5701 (5) | 0.0736 (11) | |
H4 | 0.7425 | 0.6938 | 0.6028 | 0.088* | |
C5 | 0.5950 (4) | 0.7669 (2) | 0.6178 (4) | 0.0667 (10) | |
H5 | 0.5649 | 0.7390 | 0.6838 | 0.080* | |
C12 | 0.2260 (4) | 0.9294 (3) | 0.4062 (4) | 0.0729 (11) | |
H12 | 0.2548 | 0.9145 | 0.4949 | 0.087* | |
C13 | 0.6961 (5) | 0.8024 (3) | 0.0321 (4) | 0.0731 (11) | |
C9 | 0.1401 (5) | 0.9684 (3) | 0.1490 (5) | 0.0819 (13) | |
H9 | 0.1112 | 0.9812 | 0.0593 | 0.098* | |
C11 | 0.0889 (4) | 0.9245 (3) | 0.3452 (5) | 0.0830 (13) | |
H11 | 0.0245 | 0.9081 | 0.3932 | 0.100* | |
C3 | 0.7430 (4) | 0.7802 (3) | 0.4734 (5) | 0.0757 (11) | |
H3 | 0.8154 | 0.7607 | 0.4387 | 0.091* | |
C10 | 0.0478 (4) | 0.9433 (2) | 0.2168 (5) | 0.0735 (12) | |
H10 | −0.0450 | 0.9388 | 0.1745 | 0.088* | |
F2 | 0.7758 (4) | 0.8166 (3) | −0.0462 (4) | 0.1362 (14) | |
F3 | 0.6357 (4) | 0.73743 (16) | −0.0037 (4) | 0.1363 (15) | |
F1 | 0.7723 (3) | 0.7912 (2) | 0.1497 (3) | 0.1225 (12) | |
O2 | 0.4961 (3) | 0.85106 (17) | 0.1200 (3) | 0.0738 (7) | |
O1 | 0.6587 (3) | 0.94232 (16) | 0.0761 (3) | 0.0799 (8) | |
N1 | 0.8058 (3) | 1.0888 (2) | 0.2480 (4) | 0.0730 (9) | |
C14 | 0.8980 (4) | 1.1225 (2) | 0.2413 (4) | 0.0650 (9) | |
O3 | 0.5061 (4) | 0.88004 (19) | −0.1030 (3) | 0.0885 (10) | |
C15 | 1.0188 (5) | 1.1660 (3) | 0.2352 (6) | 0.0971 (16) | |
H15A | 1.0059 | 1.2196 | 0.2572 | 0.146* | |
H15B | 1.0353 | 1.1630 | 0.1468 | 0.146* | |
H15C | 1.0966 | 1.1447 | 0.2974 | 0.146* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.05592 (17) | 0.05287 (16) | 0.05747 (17) | −0.00550 (10) | 0.02006 (12) | 0.00355 (10) |
P1 | 0.0370 (4) | 0.0361 (3) | 0.0438 (4) | −0.0028 (3) | 0.0059 (3) | 0.0003 (3) |
S3 | 0.0570 (4) | 0.0431 (4) | 0.0537 (4) | 0.0051 (3) | 0.0155 (4) | 0.0008 (3) |
C7 | 0.0388 (14) | 0.0346 (13) | 0.0553 (17) | −0.0022 (11) | 0.0039 (12) | −0.0029 (12) |
C8 | 0.0480 (18) | 0.073 (2) | 0.062 (2) | 0.0061 (16) | 0.0032 (16) | 0.0082 (17) |
C1 | 0.0421 (14) | 0.0360 (13) | 0.0508 (16) | 0.0020 (11) | 0.0018 (12) | 0.0001 (12) |
C2 | 0.0521 (18) | 0.063 (2) | 0.066 (2) | 0.0107 (16) | 0.0090 (16) | 0.0091 (17) |
C6 | 0.064 (2) | 0.0435 (16) | 0.073 (2) | 0.0015 (14) | 0.0228 (18) | 0.0042 (15) |
C4 | 0.063 (2) | 0.0495 (19) | 0.097 (3) | 0.0097 (17) | −0.007 (2) | 0.016 (2) |
C5 | 0.075 (2) | 0.0462 (18) | 0.077 (2) | −0.0031 (17) | 0.011 (2) | 0.0162 (17) |
C12 | 0.056 (2) | 0.096 (3) | 0.063 (2) | −0.024 (2) | 0.0046 (17) | 0.011 (2) |
C13 | 0.079 (3) | 0.073 (3) | 0.072 (2) | 0.023 (2) | 0.027 (2) | 0.002 (2) |
C9 | 0.056 (2) | 0.102 (4) | 0.073 (3) | 0.009 (2) | −0.016 (2) | 0.010 (2) |
C11 | 0.049 (2) | 0.094 (3) | 0.104 (3) | −0.023 (2) | 0.013 (2) | 0.012 (3) |
C3 | 0.059 (2) | 0.073 (3) | 0.094 (3) | 0.0232 (19) | 0.014 (2) | 0.009 (2) |
C10 | 0.0448 (19) | 0.062 (2) | 0.098 (3) | 0.0001 (16) | −0.017 (2) | −0.002 (2) |
F2 | 0.122 (3) | 0.182 (4) | 0.134 (3) | 0.054 (2) | 0.090 (2) | 0.022 (3) |
F3 | 0.177 (4) | 0.0536 (17) | 0.182 (4) | 0.0202 (19) | 0.046 (3) | −0.0193 (19) |
F1 | 0.102 (2) | 0.163 (3) | 0.099 (2) | 0.071 (2) | 0.0145 (17) | 0.024 (2) |
O2 | 0.0638 (16) | 0.0796 (18) | 0.0868 (19) | −0.0078 (14) | 0.0355 (15) | −0.0007 (15) |
O1 | 0.102 (2) | 0.0586 (15) | 0.090 (2) | −0.0251 (15) | 0.0457 (18) | −0.0175 (14) |
N1 | 0.0616 (19) | 0.071 (2) | 0.089 (2) | −0.0154 (16) | 0.0215 (17) | −0.0050 (18) |
C14 | 0.059 (2) | 0.068 (2) | 0.069 (2) | −0.0121 (17) | 0.0172 (18) | −0.0080 (18) |
O3 | 0.111 (2) | 0.081 (2) | 0.0627 (17) | 0.0280 (18) | −0.0042 (16) | 0.0076 (14) |
C15 | 0.068 (3) | 0.105 (4) | 0.123 (4) | −0.028 (3) | 0.031 (3) | −0.007 (3) |
Ag1—N1 | 2.242 (3) | C4—C5 | 1.344 (6) |
Ag1—P1 | 2.4068 (8) | C4—C3 | 1.383 (6) |
Ag1—O1 | 2.455 (3) | C4—H4 | 0.9500 |
Ag1—O3i | 2.470 (3) | C5—H5 | 0.9500 |
P1—C7 | 1.824 (3) | C12—C11 | 1.398 (5) |
P1—C1 | 1.832 (3) | C12—H12 | 0.9500 |
P1—P1ii | 2.2206 (15) | C13—F2 | 1.295 (5) |
S3—O3 | 1.427 (3) | C13—F3 | 1.305 (5) |
S3—O2 | 1.429 (3) | C13—F1 | 1.320 (5) |
S3—O1 | 1.433 (3) | C9—C10 | 1.365 (7) |
S3—C13 | 1.799 (4) | C9—H9 | 0.9500 |
C7—C8 | 1.378 (5) | C11—C10 | 1.362 (7) |
C7—C12 | 1.378 (5) | C11—H11 | 0.9500 |
C8—C9 | 1.392 (6) | C3—H3 | 0.9500 |
C8—H8 | 0.9500 | C10—H10 | 0.9500 |
C1—C6 | 1.378 (5) | N1—C14 | 1.118 (5) |
C1—C2 | 1.394 (5) | C14—C15 | 1.452 (6) |
C2—C3 | 1.383 (5) | O3—Ag1i | 2.470 (3) |
C2—H2 | 0.9500 | C15—H15A | 0.9800 |
C6—C5 | 1.396 (5) | C15—H15B | 0.9800 |
C6—H6 | 0.9500 | C15—H15C | 0.9800 |
N1—Ag1—P1 | 140.60 (10) | C3—C4—H4 | 119.9 |
N1—Ag1—O1 | 88.97 (11) | C4—C5—C6 | 120.6 (4) |
P1—Ag1—O1 | 118.38 (7) | C4—C5—H5 | 119.7 |
N1—Ag1—O3i | 86.61 (13) | C6—C5—H5 | 119.7 |
P1—Ag1—O3i | 117.23 (9) | C7—C12—C11 | 120.8 (4) |
O1—Ag1—O3i | 92.72 (11) | C7—C12—H12 | 119.6 |
C7—P1—C1 | 109.67 (13) | C11—C12—H12 | 119.6 |
C7—P1—P1ii | 102.26 (11) | F2—C13—F3 | 107.5 (4) |
C1—P1—P1ii | 101.08 (11) | F2—C13—F1 | 107.8 (4) |
C7—P1—Ag1 | 111.71 (11) | F3—C13—F1 | 106.4 (4) |
C1—P1—Ag1 | 113.08 (11) | F2—C13—S3 | 112.0 (3) |
P1ii—P1—Ag1 | 118.02 (5) | F3—C13—S3 | 110.9 (3) |
O3—S3—O2 | 115.9 (2) | F1—C13—S3 | 111.9 (3) |
O3—S3—O1 | 115.4 (2) | C10—C9—C8 | 120.6 (4) |
O2—S3—O1 | 114.45 (17) | C10—C9—H9 | 119.7 |
O3—S3—C13 | 102.2 (2) | C8—C9—H9 | 119.7 |
O2—S3—C13 | 103.52 (19) | C10—C11—C12 | 119.8 (4) |
O1—S3—C13 | 102.6 (2) | C10—C11—H11 | 120.1 |
C8—C7—C12 | 118.5 (3) | C12—C11—H11 | 120.1 |
C8—C7—P1 | 116.4 (3) | C4—C3—C2 | 120.1 (4) |
C12—C7—P1 | 125.0 (3) | C4—C3—H3 | 119.9 |
C7—C8—C9 | 120.3 (4) | C2—C3—H3 | 119.9 |
C7—C8—H8 | 119.8 | C11—C10—C9 | 119.9 (4) |
C9—C8—H8 | 119.8 | C11—C10—H10 | 120.0 |
C6—C1—C2 | 118.7 (3) | C9—C10—H10 | 120.0 |
C6—C1—P1 | 124.7 (2) | S3—O1—Ag1 | 121.18 (17) |
C2—C1—P1 | 116.6 (3) | C14—N1—Ag1 | 177.9 (4) |
C3—C2—C1 | 120.1 (4) | N1—C14—C15 | 178.9 (5) |
C3—C2—H2 | 120.0 | S3—O3—Ag1i | 136.42 (19) |
C1—C2—H2 | 120.0 | C14—C15—H15A | 109.5 |
C1—C6—C5 | 120.3 (3) | C14—C15—H15B | 109.5 |
C1—C6—H6 | 119.9 | H15A—C15—H15B | 109.5 |
C5—C6—H6 | 119.9 | C14—C15—H15C | 109.5 |
C5—C4—C3 | 120.1 (3) | H15A—C15—H15C | 109.5 |
C5—C4—H4 | 119.9 | H15B—C15—H15C | 109.5 |
Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag2(CF3SO3)2(C28H26N2P2)] |
Mr | 483.16 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 105 |
a, b, c (Å) | 10.1128 (2), 17.4753 (3), 10.5053 (2) |
β (°) | 102.599 (1) |
V (Å3) | 1811.84 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.36 |
Crystal size (mm) | 0.21 × 0.17 × 0.10 |
Data collection | |
Diffractometer | Bruker X8 APEX |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.760, 0.873 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 28681, 4502, 3588 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.668 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.112, 1.04 |
No. of reflections | 4502 |
No. of parameters | 227 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.47, −0.23 |
Computer programs: APEX2 (Bruker, 2003), SAINT-Plus (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2003).
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The title polymer contains AgI ions in pseudo tetrahedral geometry bridged by a rigid bidentate diphosphine (DPP) ligand (Klausmeyer et al., 2004). The distorted tetrahedral angles range from 140.60 (10) to 86.61 (13)°. The AgI ion is stabilized by the soft donor phosphorus, from DPP, and 2 hard oxo ligands, from trifluoromethanesulfonate. The structure contains an 8-membered ring containing the silvers and the anions (Fig. 1). This ring is situated on an inversion center. The rings are then linked by the diphosphine ligand through the silvers into a one-dimensional polymer which boasts a 'Ring—P—P—Ring' design resembling a staircase (Fig. 2). The extended packing structure indicates that F atoms on the trifluoromethanesulfonate ion form a 3.186 (4) Å interaction with a C—H group on a neighboring 'staircase' polymer.