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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804031435/hb6097sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804031435/hb6097Isup2.hkl
Contains datablock I

CCDC reference: 262229

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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)]·2H2OF(000) = 792
Mr = 397.07Dx = 1.904 Mg m3
Monoclinic, P2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ycCell parameters from 25 reflections
a = 8.566 (6) Åθ = 4–27°
b = 8.807 (7) ŵ = 1.60 mm1
c = 18.729 (17) ÅT = 293 K
β = 101.37°Needle, colourless
V = 1385.2 (19) Å30.20 × 0.10 × 0.08 mm
Z = 4
Data collection top
Siemens R3m
diffractometer
1618 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.028
Graphite monochromatorθmax = 28.0°, θmin = 2.3°
ω scansh = 010
Absorption correction: ψ scan
(North et al., 1968)
k = 011
Tmin = 0.843, Tmax = 0.880l = 2424
3174 measured reflections2 standard reflections every 118 reflections
2939 independent reflections intensity decay: none
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)] = 0.091Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.328H-atom parameters constrained
S = 1.09
2939 reflections(Δ/σ)max = 0.001
171 parametersΔρmax = 1.59 e Å3
2 restraintsΔρmin = 1.08 e Å3
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
Ag10.79709 (13)0.07361 (15)0.51662 (5)0.0931 (6)
P10.7557 (4)0.4906 (5)0.5049 (2)0.0793 (9)
O10.8587 (11)0.3610 (11)0.4933 (6)0.098 (3)
O20.6775 (13)0.4557 (17)0.5717 (6)0.128 (5)
H2A0.57750.46870.55930.080*
O30.8534 (13)0.6392 (14)0.5236 (7)0.116 (4)
H3A0.94690.62550.51580.080*
O40.6213 (12)0.5214 (14)0.4381 (5)0.099 (3)
N10.5979 (14)0.0365 (13)0.4288 (6)0.081 (3)
N20.0130 (16)0.0487 (15)0.1112 (6)0.092 (3)
C10.5439 (16)0.1025 (16)0.4030 (7)0.080 (3)
H1B0.59080.19060.42890.080*
C20.4273 (19)0.1216 (18)0.3430 (8)0.090 (4)
H2B0.39780.22290.32670.080*
C30.3509 (15)0.0000 (16)0.3052 (6)0.071 (3)
C40.402 (2)0.1413 (18)0.3314 (8)0.098 (4)
H4A0.35340.23050.30730.080*
C50.5233 (19)0.1589 (19)0.3924 (8)0.099 (4)
H5A0.55650.25880.40950.080*
C60.2244 (14)0.0186 (15)0.2381 (6)0.071 (3)
C70.1759 (19)0.1576 (19)0.2104 (8)0.100 (4)
H7A0.22380.24760.23400.080*
C80.0606 (19)0.1718 (18)0.1477 (8)0.097 (4)
H8A0.02950.27080.12860.080*
C90.038 (2)0.0873 (16)0.1389 (9)0.091 (4)
H9A0.00900.17560.11340.080*
C100.1492 (19)0.104 (2)0.2015 (8)0.097 (4)
H10A0.17760.20470.21920.080*
O2W0.628 (3)0.511 (3)0.7928 (11)0.215 (8)*
H2WA0.59050.59950.78320.080*
H2WB0.72890.52820.79710.050*
O1W0.1193 (12)0.499 (5)0.2602 (13)0.42 (2)*
H1WA0.06440.46600.29150.050*
H1WB0.21630.47990.28220.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.0918 (8)0.1300 (11)0.0572 (6)0.0048 (6)0.0140 (5)0.0002 (6)
P10.0782 (18)0.096 (2)0.0712 (19)0.0035 (17)0.0331 (15)0.0049 (18)
O10.078 (5)0.085 (6)0.138 (9)0.021 (5)0.041 (5)0.007 (6)
O20.086 (6)0.231 (15)0.072 (6)0.006 (7)0.031 (5)0.035 (8)
O30.087 (6)0.119 (8)0.150 (10)0.022 (6)0.039 (6)0.071 (8)
O40.094 (6)0.142 (9)0.069 (5)0.014 (6)0.039 (5)0.012 (6)
N10.096 (7)0.089 (8)0.063 (6)0.007 (6)0.028 (5)0.011 (5)
N20.112 (8)0.108 (9)0.063 (6)0.010 (7)0.039 (6)0.002 (6)
C10.095 (8)0.084 (9)0.059 (6)0.004 (6)0.012 (6)0.003 (6)
C20.116 (10)0.091 (9)0.064 (7)0.011 (8)0.021 (7)0.010 (6)
C30.083 (7)0.079 (7)0.052 (6)0.001 (6)0.015 (5)0.007 (6)
C40.123 (11)0.076 (8)0.086 (9)0.000 (8)0.001 (8)0.010 (8)
C50.108 (10)0.091 (9)0.089 (10)0.016 (8)0.000 (8)0.004 (8)
C60.082 (7)0.084 (8)0.047 (5)0.004 (6)0.016 (5)0.007 (5)
C70.125 (11)0.089 (9)0.076 (8)0.001 (9)0.007 (8)0.011 (8)
C80.124 (11)0.073 (8)0.087 (9)0.004 (8)0.005 (8)0.002 (7)
C90.128 (12)0.070 (8)0.081 (9)0.009 (8)0.034 (8)0.010 (7)
C100.102 (10)0.110 (12)0.076 (9)0.002 (8)0.007 (7)0.009 (8)
Geometric parameters (Å, º) top
Ag1—N12.148 (12)C3—C41.38 (2)
Ag1—N2i2.168 (14)C3—C61.496 (17)
Ag1—O12.639 (10)C4—C51.39 (2)
P1—O11.485 (11)C4—H4A0.9600
P1—O41.548 (11)C5—H5A0.9599
P1—O31.556 (12)C6—C71.36 (2)
P1—O21.562 (10)C6—C101.371 (19)
O2—H2A0.8500C7—C81.38 (2)
O3—H3A0.8500C7—H7A0.9600
N1—C11.363 (18)C8—H8A0.9600
N1—C51.365 (19)C9—C101.36 (2)
N2—C91.344 (19)C9—H9A0.9599
N2—C81.367 (19)C10—H10A0.9600
N2—Ag1ii2.168 (14)O2W—H2WA0.8500
C1—C21.36 (2)O2W—H2WB0.8671
C1—H1B0.9600O1W—H1WA0.8715
C2—C31.377 (19)O1W—H1WB0.8684
C2—H2B0.9600
N1—Ag1—N2i164.8 (5)C4—C3—C6121.7 (12)
N1—Ag1—O1100.0 (4)C3—C4—C5121.8 (14)
N2i—Ag1—O195.2 (2)C3—C4—H4A119.5
O1—P1—O4112.7 (6)C5—C4—H4A118.7
O1—P1—O3111.8 (6)N1—C5—C4121.5 (15)
O4—P1—O3108.4 (7)N1—C5—H5A118.6
O1—P1—O2109.1 (7)C4—C5—H5A120.0
O4—P1—O2108.3 (6)C7—C6—C10116.1 (13)
O3—P1—O2106.4 (7)C7—C6—C3122.3 (12)
P1—O2—H2A108.9C10—C6—C3121.6 (13)
P1—O3—H3A109.0C6—C7—C8121.2 (14)
C1—N1—C5116.0 (12)C6—C7—H7A119.7
C1—N1—Ag1124.8 (9)C8—C7—H7A119.1
C5—N1—Ag1119.0 (10)N2—C8—C7122.3 (15)
C9—N2—C8115.5 (14)N2—C8—H8A117.9
C9—N2—Ag1ii122.8 (10)C7—C8—H8A119.8
C8—N2—Ag1ii121.7 (11)N2—C9—C10123.3 (15)
C2—C1—N1123.2 (13)N2—C9—H9A117.1
C2—C1—H1B118.9C10—C9—H9A119.6
N1—C1—H1B117.9C9—C10—C6121.5 (15)
C1—C2—C3121.8 (15)C9—C10—H10A118.9
C1—C2—H2B118.9C6—C10—H10A119.5
C3—C2—H2B119.3H2WA—O2W—H2WB100.6
C2—C3—C4115.6 (13)H1WA—O1W—H1WB102.0
C2—C3—C6122.6 (14)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x1, y, z1/2.
 

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