The crystal structure of the title complex, {[Ag(H2PO4)(C10H8N2)]·2H2O}n, reveals a T-shaped geometry for the AgI atom [N—Ag—N = 164.8 (5)°, and O—Ag—N = 100.0 (4) and 95.2 (2)°], coordinated by two N atoms from two 4,4′-bipyridine molecules and an O atom from a H2PO4− counter-ion. The silver–4,4′-bipyridine connectivity results in polymeric chains.
Supporting information
CCDC reference: 262229
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.020 Å
- R factor = 0.091
- wR factor = 0.328
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.82
Alert level B
REFLT03_ALERT_3_B Reflection count < 90% complete (theta max?)
From the CIF: _diffrn_reflns_theta_max 28.01
From the CIF: _diffrn_reflns_theta_full 0.00
From the CIF: _reflns_number_total 2939
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 3361
Completeness (_total/calc) 87.44%
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for P1
PLAT417_ALERT_2_B Short Inter D-H..H-D H1WA .. H1WA .. 1.72 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WA .. H2WA .. 1.79 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WB .. H1WB .. 1.65 Ang.
Alert level C
RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25
Weighted R factor given 0.328
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT084_ALERT_2_C High R2 Value .................................. 0.33
PLAT145_ALERT_4_C su on beta Small or Missing (x 10000) ..... 0 Deg.
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 2
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C10
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 20
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
1 ALERT level A = In general: serious problem
5 ALERT level B = Potentially serious problem
10 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
8 ALERT type 2 Indicator that the structure model may be wrong or deficient
5 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: R3m Software (Siemens, 1990); cell refinement: R3m Software; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXL97.
catena-Poly[[(dihydrogenphosphato)silver(I)]-µ-4,4'-bipyridine]
dihydrate]
top
Crystal data top
[Ag(H2PO4)(C10H8N2)]·2H2O | F(000) = 792 |
Mr = 397.07 | Dx = 1.904 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 25 reflections |
a = 8.566 (6) Å | θ = 4–27° |
b = 8.807 (7) Å | µ = 1.60 mm−1 |
c = 18.729 (17) Å | T = 293 K |
β = 101.37° | Needle, colourless |
V = 1385.2 (19) Å3 | 0.20 × 0.10 × 0.08 mm |
Z = 4 | |
Data collection top
Siemens R3m diffractometer | 1618 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 28.0°, θmin = 2.3° |
ω scans | h = 0→10 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→11 |
Tmin = 0.843, Tmax = 0.880 | l = −24→24 |
3174 measured reflections | 2 standard reflections every 118 reflections |
2939 independent reflections | intensity decay: none |
Refinement top
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)] = 0.091 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.328 | H-atom parameters constrained |
S = 1.09 | |
2939 reflections | (Δ/σ)max = 0.001 |
171 parameters | Δρmax = 1.59 e Å−3 |
2 restraints | Δρmin = −1.08 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Ag1 | 0.79709 (13) | 0.07361 (15) | 0.51662 (5) | 0.0931 (6) | |
P1 | 0.7557 (4) | 0.4906 (5) | 0.5049 (2) | 0.0793 (9) | |
O1 | 0.8587 (11) | 0.3610 (11) | 0.4933 (6) | 0.098 (3) | |
O2 | 0.6775 (13) | 0.4557 (17) | 0.5717 (6) | 0.128 (5) | |
H2A | 0.5775 | 0.4687 | 0.5593 | 0.080* | |
O3 | 0.8534 (13) | 0.6392 (14) | 0.5236 (7) | 0.116 (4) | |
H3A | 0.9469 | 0.6255 | 0.5158 | 0.080* | |
O4 | 0.6213 (12) | 0.5214 (14) | 0.4381 (5) | 0.099 (3) | |
N1 | 0.5979 (14) | 0.0365 (13) | 0.4288 (6) | 0.081 (3) | |
N2 | −0.0130 (16) | −0.0487 (15) | 0.1112 (6) | 0.092 (3) | |
C1 | 0.5439 (16) | −0.1025 (16) | 0.4030 (7) | 0.080 (3) | |
H1B | 0.5908 | −0.1906 | 0.4289 | 0.080* | |
C2 | 0.4273 (19) | −0.1216 (18) | 0.3430 (8) | 0.090 (4) | |
H2B | 0.3978 | −0.2229 | 0.3267 | 0.080* | |
C3 | 0.3509 (15) | 0.0000 (16) | 0.3052 (6) | 0.071 (3) | |
C4 | 0.402 (2) | 0.1413 (18) | 0.3314 (8) | 0.098 (4) | |
H4A | 0.3534 | 0.2305 | 0.3073 | 0.080* | |
C5 | 0.5233 (19) | 0.1589 (19) | 0.3924 (8) | 0.099 (4) | |
H5A | 0.5565 | 0.2588 | 0.4095 | 0.080* | |
C6 | 0.2244 (14) | −0.0186 (15) | 0.2381 (6) | 0.071 (3) | |
C7 | 0.1759 (19) | −0.1576 (19) | 0.2104 (8) | 0.100 (4) | |
H7A | 0.2238 | −0.2476 | 0.2340 | 0.080* | |
C8 | 0.0606 (19) | −0.1718 (18) | 0.1477 (8) | 0.097 (4) | |
H8A | 0.0295 | −0.2708 | 0.1286 | 0.080* | |
C9 | 0.038 (2) | 0.0873 (16) | 0.1389 (9) | 0.091 (4) | |
H9A | −0.0090 | 0.1756 | 0.1134 | 0.080* | |
C10 | 0.1492 (19) | 0.104 (2) | 0.2015 (8) | 0.097 (4) | |
H10A | 0.1776 | 0.2047 | 0.2192 | 0.080* | |
O2W | 0.628 (3) | 0.511 (3) | 0.7928 (11) | 0.215 (8)* | |
H2WA | 0.5905 | 0.5995 | 0.7832 | 0.080* | |
H2WB | 0.7289 | 0.5282 | 0.7971 | 0.050* | |
O1W | 0.1193 (12) | 0.499 (5) | 0.2602 (13) | 0.42 (2)* | |
H1WA | 0.0644 | 0.4660 | 0.2915 | 0.050* | |
H1WB | 0.2163 | 0.4799 | 0.2822 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.0918 (8) | 0.1300 (11) | 0.0572 (6) | −0.0048 (6) | 0.0140 (5) | 0.0002 (6) |
P1 | 0.0782 (18) | 0.096 (2) | 0.0712 (19) | −0.0035 (17) | 0.0331 (15) | −0.0049 (18) |
O1 | 0.078 (5) | 0.085 (6) | 0.138 (9) | −0.021 (5) | 0.041 (5) | −0.007 (6) |
O2 | 0.086 (6) | 0.231 (15) | 0.072 (6) | −0.006 (7) | 0.031 (5) | 0.035 (8) |
O3 | 0.087 (6) | 0.119 (8) | 0.150 (10) | −0.022 (6) | 0.039 (6) | −0.071 (8) |
O4 | 0.094 (6) | 0.142 (9) | 0.069 (5) | 0.014 (6) | 0.039 (5) | 0.012 (6) |
N1 | 0.096 (7) | 0.089 (8) | 0.063 (6) | 0.007 (6) | 0.028 (5) | 0.011 (5) |
N2 | 0.112 (8) | 0.108 (9) | 0.063 (6) | 0.010 (7) | 0.039 (6) | 0.002 (6) |
C1 | 0.095 (8) | 0.084 (9) | 0.059 (6) | 0.004 (6) | 0.012 (6) | 0.003 (6) |
C2 | 0.116 (10) | 0.091 (9) | 0.064 (7) | 0.011 (8) | 0.021 (7) | 0.010 (6) |
C3 | 0.083 (7) | 0.079 (7) | 0.052 (6) | −0.001 (6) | 0.015 (5) | 0.007 (6) |
C4 | 0.123 (11) | 0.076 (8) | 0.086 (9) | 0.000 (8) | −0.001 (8) | 0.010 (8) |
C5 | 0.108 (10) | 0.091 (9) | 0.089 (10) | −0.016 (8) | 0.000 (8) | 0.004 (8) |
C6 | 0.082 (7) | 0.084 (8) | 0.047 (5) | 0.004 (6) | 0.016 (5) | 0.007 (5) |
C7 | 0.125 (11) | 0.089 (9) | 0.076 (8) | 0.001 (9) | −0.007 (8) | 0.011 (8) |
C8 | 0.124 (11) | 0.073 (8) | 0.087 (9) | 0.004 (8) | 0.005 (8) | 0.002 (7) |
C9 | 0.128 (12) | 0.070 (8) | 0.081 (9) | 0.009 (8) | 0.034 (8) | 0.010 (7) |
C10 | 0.102 (10) | 0.110 (12) | 0.076 (9) | 0.002 (8) | 0.007 (7) | −0.009 (8) |
Geometric parameters (Å, º) top
Ag1—N1 | 2.148 (12) | C3—C4 | 1.38 (2) |
Ag1—N2i | 2.168 (14) | C3—C6 | 1.496 (17) |
Ag1—O1 | 2.639 (10) | C4—C5 | 1.39 (2) |
P1—O1 | 1.485 (11) | C4—H4A | 0.9600 |
P1—O4 | 1.548 (11) | C5—H5A | 0.9599 |
P1—O3 | 1.556 (12) | C6—C7 | 1.36 (2) |
P1—O2 | 1.562 (10) | C6—C10 | 1.371 (19) |
O2—H2A | 0.8500 | C7—C8 | 1.38 (2) |
O3—H3A | 0.8500 | C7—H7A | 0.9600 |
N1—C1 | 1.363 (18) | C8—H8A | 0.9600 |
N1—C5 | 1.365 (19) | C9—C10 | 1.36 (2) |
N2—C9 | 1.344 (19) | C9—H9A | 0.9599 |
N2—C8 | 1.367 (19) | C10—H10A | 0.9600 |
N2—Ag1ii | 2.168 (14) | O2W—H2WA | 0.8500 |
C1—C2 | 1.36 (2) | O2W—H2WB | 0.8671 |
C1—H1B | 0.9600 | O1W—H1WA | 0.8715 |
C2—C3 | 1.377 (19) | O1W—H1WB | 0.8684 |
C2—H2B | 0.9600 | | |
| | | |
N1—Ag1—N2i | 164.8 (5) | C4—C3—C6 | 121.7 (12) |
N1—Ag1—O1 | 100.0 (4) | C3—C4—C5 | 121.8 (14) |
N2i—Ag1—O1 | 95.2 (2) | C3—C4—H4A | 119.5 |
O1—P1—O4 | 112.7 (6) | C5—C4—H4A | 118.7 |
O1—P1—O3 | 111.8 (6) | N1—C5—C4 | 121.5 (15) |
O4—P1—O3 | 108.4 (7) | N1—C5—H5A | 118.6 |
O1—P1—O2 | 109.1 (7) | C4—C5—H5A | 120.0 |
O4—P1—O2 | 108.3 (6) | C7—C6—C10 | 116.1 (13) |
O3—P1—O2 | 106.4 (7) | C7—C6—C3 | 122.3 (12) |
P1—O2—H2A | 108.9 | C10—C6—C3 | 121.6 (13) |
P1—O3—H3A | 109.0 | C6—C7—C8 | 121.2 (14) |
C1—N1—C5 | 116.0 (12) | C6—C7—H7A | 119.7 |
C1—N1—Ag1 | 124.8 (9) | C8—C7—H7A | 119.1 |
C5—N1—Ag1 | 119.0 (10) | N2—C8—C7 | 122.3 (15) |
C9—N2—C8 | 115.5 (14) | N2—C8—H8A | 117.9 |
C9—N2—Ag1ii | 122.8 (10) | C7—C8—H8A | 119.8 |
C8—N2—Ag1ii | 121.7 (11) | N2—C9—C10 | 123.3 (15) |
C2—C1—N1 | 123.2 (13) | N2—C9—H9A | 117.1 |
C2—C1—H1B | 118.9 | C10—C9—H9A | 119.6 |
N1—C1—H1B | 117.9 | C9—C10—C6 | 121.5 (15) |
C1—C2—C3 | 121.8 (15) | C9—C10—H10A | 118.9 |
C1—C2—H2B | 118.9 | C6—C10—H10A | 119.5 |
C3—C2—H2B | 119.3 | H2WA—O2W—H2WB | 100.6 |
C2—C3—C4 | 115.6 (13) | H1WA—O1W—H1WB | 102.0 |
C2—C3—C6 | 122.6 (14) | | |
Symmetry codes: (i) x+1, −y, z+1/2; (ii) x−1, −y, z−1/2. |