In the crystal structure of {[Ag(BrO
3)(C
10H
8N
2)]·2.5H
2O}
n, the Ag atom is coordinated by the N atoms of two different spacer donor ligands [Ag—N = 2.147 (2) and 2.152 (2) Å, and N—Ag—N = 172.0 (1)°], but is connected only weakly to the O atoms of two different bromate counter-ions [Ag—O = 2.877 (3) and 2.972 (3) Å, and O—Ag—O = 162.3 (1)°]; the coordination geometry of the Ag atom is approximately planar. The (C
10H
8N
2)Ag chains, which propagate along [10
], are cross-linked in the
b direction by bromate anions and Ag
Ag [3.3197 (6) Å] interactions, thus forming sheets.
Supporting information
CCDC reference: 238631
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.004 Å
- R factor = 0.030
- wR factor = 0.084
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... Br1
PLAT417_ALERT_2_B Short Inter D-H..H-D H2W1 .. H2W1 .. 1.83 Ang.
PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.864(10) ...... 5.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT731_ALERT_1_B Bond Calc 0.87(5), Rep 0.870(10) ...... 5.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.864(10) ...... 5.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.860(10) ...... 5.00 su-Rat
O1W -H2# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.87(5), Rep 0.870(10) ...... 5.00 su-Rat
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.860(10) ...... 5.00 su-Rat
O2W -H4# 1.555 1.555
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.201 0.416
Tmin' and Tmax expected: 0.185 0.345
RR' = 0.900
Please check that your absorption correction is appropriate.
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.83
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.83
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.11
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.862(10) ...... 4.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 107(4), Rep 107.1(17) ...... 2.35 su-Rat
H1W1 -O1W -H1W2 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 106(5), Rep 105.7(17) ...... 2.94 su-Rat
H2W1 -O2W -H2W2 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.860(10) ...... 4.00 su-Rat
O1W -H1# 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.22 Ratio
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C10 H13 Ag1 Br1 N2 O5.5
Atom count from _chemical_formula_moiety:C10 H13 Ag1 Br1 N2 O32.5
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.830
Tmax scaled 0.345 Tmin scaled 0.167
0 ALERT level A = In general: serious problem
8 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
14 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[[bromatosilver(I)-µ-4,4'-bipyridine] 2.5-hydrate]
top
Crystal data top
[Ag(BrO3)(C10H8N2)]·2.5H2O | F(000) = 852 |
Mr = 437.00 | Dx = 2.128 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4053 reflections |
a = 13.1128 (8) Å | θ = 2.4–28.2° |
b = 6.9843 (4) Å | µ = 4.43 mm−1 |
c = 15.3908 (9) Å | T = 298 K |
β = 104.647 (1)° | Column, colorless |
V = 1363.74 (14) Å3 | 0.37 × 0.25 × 0.24 mm |
Z = 4 | |
Data collection top
Bruker APEX area-detector diffractometer | 3066 independent reflections |
Radiation source: fine-focus sealed tube | 2650 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scan | θmax = 27.5°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −14→16 |
Tmin = 0.201, Tmax = 0.416 | k = −7→9 |
7759 measured reflections | l = −19→19 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0534P)2 + 0.025P] where P = (Fo2 + 2Fc2)/3 |
3066 reflections | (Δ/σ)max = 0.001 |
196 parameters | Δρmax = 0.67 e Å−3 |
9 restraints | Δρmin = −0.77 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ag1 | −0.029037 (19) | 1.22818 (4) | 0.512076 (16) | 0.04481 (11) | |
Br1 | 0.24221 (2) | 0.90876 (5) | 0.687253 (18) | 0.04126 (11) | |
O1 | 0.1424 (2) | 1.0416 (5) | 0.6374 (2) | 0.0765 (9) | |
O2 | 0.2229 (2) | 0.7032 (4) | 0.63352 (18) | 0.0638 (7) | |
O3 | 0.3442 (2) | 1.0075 (5) | 0.6621 (2) | 0.0782 (9) | |
O1w | 0.3858 (3) | 0.4166 (7) | 0.6336 (4) | 0.1110 (13) | |
H1w1 | 0.437 (3) | 0.496 (6) | 0.638 (5) | 0.133* | |
H1w2 | 0.335 (3) | 0.479 (7) | 0.647 (5) | 0.133* | |
O2w | 0.5197 (4) | 0.1357 (9) | 0.4411 (3) | 0.1181 (15) | |
H2w1 | 0.552 (5) | 0.043 (7) | 0.475 (3) | 0.142* | |
H2w2 | 0.541 (5) | 0.132 (9) | 0.393 (3) | 0.142* | |
O3w | 0.5000 | 0.5000 | 0.5000 | 0.156 (3) | |
H3w1 | 0.496 (18) | 0.396 (18) | 0.527 (14) | 0.187* | 0.50 |
H3w2 | 0.554 (9) | 0.56 (3) | 0.528 (13) | 0.187* | 0.50 |
N1 | −0.12038 (18) | 1.1979 (3) | 0.60900 (15) | 0.0312 (5) | |
N2 | −0.42709 (18) | 1.2083 (4) | 0.92607 (15) | 0.0325 (5) | |
C1 | −0.2248 (2) | 1.2329 (4) | 0.58523 (19) | 0.0334 (6) | |
H1 | −0.2567 | 1.2625 | 0.5256 | 0.040* | |
C2 | −0.2864 (2) | 1.2267 (4) | 0.64597 (18) | 0.0298 (6) | |
H2 | −0.3583 | 1.2509 | 0.6270 | 0.036* | |
C3 | −0.24043 (19) | 1.1841 (4) | 0.73521 (15) | 0.0236 (5) | |
C4 | −0.13304 (19) | 1.1463 (4) | 0.75920 (17) | 0.0285 (5) | |
H4 | −0.0995 | 1.1161 | 0.8184 | 0.034* | |
C5 | −0.0763 (2) | 1.1534 (4) | 0.69566 (18) | 0.0316 (6) | |
H5 | −0.0046 | 1.1265 | 0.7130 | 0.038* | |
C6 | −0.4693 (2) | 1.1531 (4) | 0.84139 (19) | 0.0340 (6) | |
H6 | −0.5407 | 1.1226 | 0.8244 | 0.041* | |
C7 | −0.41121 (19) | 1.1396 (4) | 0.77813 (17) | 0.0286 (5) | |
H7 | −0.4433 | 1.1008 | 0.7198 | 0.034* | |
C8 | −0.30410 (19) | 1.1847 (4) | 0.80251 (16) | 0.0239 (5) | |
C9 | −0.2606 (2) | 1.2366 (4) | 0.89162 (18) | 0.0305 (6) | |
H9 | −0.1891 | 1.2639 | 0.9113 | 0.037* | |
C10 | −0.3239 (2) | 1.2471 (4) | 0.95023 (18) | 0.0329 (6) | |
H10 | −0.2937 | 1.2829 | 1.0093 | 0.040* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.04628 (17) | 0.05660 (18) | 0.04451 (16) | −0.00313 (10) | 0.03546 (12) | 0.00064 (10) |
Br1 | 0.03603 (18) | 0.0553 (2) | 0.03380 (17) | 0.00055 (12) | 0.01128 (12) | −0.00039 (12) |
O1 | 0.0561 (17) | 0.102 (2) | 0.0773 (18) | 0.0303 (15) | 0.0278 (14) | 0.0340 (17) |
O2 | 0.0678 (17) | 0.0637 (17) | 0.0616 (16) | −0.0100 (13) | 0.0196 (13) | −0.0159 (13) |
O3 | 0.0446 (15) | 0.094 (2) | 0.103 (2) | −0.0260 (15) | 0.0312 (15) | −0.0179 (19) |
O1w | 0.088 (3) | 0.114 (3) | 0.128 (3) | 0.000 (2) | 0.020 (3) | −0.007 (3) |
O2w | 0.092 (3) | 0.187 (5) | 0.079 (2) | 0.018 (3) | 0.029 (2) | 0.019 (3) |
O3w | 0.108 (6) | 0.217 (12) | 0.123 (7) | 0.003 (6) | −0.008 (5) | −0.001 (7) |
N1 | 0.0318 (12) | 0.0361 (12) | 0.0321 (12) | −0.0023 (9) | 0.0201 (9) | −0.0033 (10) |
N2 | 0.0302 (12) | 0.0432 (13) | 0.0311 (11) | 0.0053 (10) | 0.0209 (10) | 0.0008 (10) |
C1 | 0.0338 (15) | 0.0422 (16) | 0.0270 (13) | 0.0010 (11) | 0.0129 (11) | 0.0011 (11) |
C2 | 0.0280 (13) | 0.0383 (15) | 0.0262 (12) | 0.0032 (10) | 0.0128 (10) | 0.0004 (10) |
C3 | 0.0247 (12) | 0.0254 (12) | 0.0242 (12) | 0.0004 (9) | 0.0124 (9) | −0.0019 (9) |
C4 | 0.0240 (12) | 0.0365 (14) | 0.0269 (12) | 0.0008 (10) | 0.0099 (10) | 0.0013 (11) |
C5 | 0.0248 (13) | 0.0370 (15) | 0.0368 (14) | −0.0004 (11) | 0.0150 (11) | −0.0010 (12) |
C6 | 0.0247 (13) | 0.0410 (16) | 0.0409 (14) | −0.0017 (11) | 0.0172 (11) | −0.0017 (12) |
C7 | 0.0242 (12) | 0.0366 (14) | 0.0271 (12) | −0.0004 (10) | 0.0101 (10) | −0.0011 (11) |
C8 | 0.0248 (12) | 0.0259 (12) | 0.0242 (11) | 0.0020 (9) | 0.0120 (9) | 0.0014 (10) |
C9 | 0.0232 (13) | 0.0421 (16) | 0.0282 (13) | 0.0015 (10) | 0.0104 (10) | −0.0007 (10) |
C10 | 0.0320 (15) | 0.0463 (17) | 0.0238 (12) | 0.0039 (11) | 0.0131 (11) | −0.0038 (11) |
Geometric parameters (Å, º) top
Ag1—N1 | 2.147 (2) | N2—Ag1iii | 2.152 (2) |
Ag1—N2i | 2.152 (2) | C1—C2 | 1.382 (4) |
Ag1—O1 | 2.877 (3) | C1—H1 | 0.9300 |
Ag1—O2ii | 2.972 (3) | C2—C3 | 1.385 (4) |
Ag1—Ag1ii | 3.3197 (6) | C2—H2 | 0.9300 |
Br1—O1 | 1.629 (3) | C3—C4 | 1.388 (3) |
Br1—O3 | 1.637 (3) | C3—C8 | 1.486 (3) |
Br1—O2 | 1.644 (3) | C4—C5 | 1.371 (3) |
O1w—H1w1 | 0.862 (10) | C4—H4 | 0.9300 |
O1w—H1w2 | 0.864 (10) | C5—H5 | 0.9300 |
O2w—H2w1 | 0.870 (10) | C6—C7 | 1.383 (3) |
O2w—H2w2 | 0.864 (10) | C6—H6 | 0.9300 |
O3w—H3w1 | 0.849 (10) | C7—C8 | 1.395 (3) |
O3w—H3w2 | 0.848 (10) | C7—H7 | 0.9300 |
N1—C1 | 1.347 (4) | C8—C9 | 1.393 (4) |
N1—C5 | 1.349 (4) | C9—C10 | 1.373 (4) |
N2—C10 | 1.337 (4) | C9—H9 | 0.9300 |
N2—C6 | 1.338 (4) | C10—H10 | 0.9300 |
| | | |
N1—Ag1—N2i | 172.0 (1) | C1—C2—H2 | 120.1 |
N1—Ag1—O1 | 88.2 (1) | C3—C2—H2 | 120.1 |
N1—Ag1—O2ii | 91.1 (1) | C2—C3—C4 | 117.5 (2) |
N2i—Ag1—O1 | 90.3 (1) | C2—C3—C8 | 120.7 (2) |
N2i—Ag1—O2ii | 92.81 (9) | C4—C3—C8 | 121.8 (2) |
O1—Ag1—O2ii | 162.3 (1) | C5—C4—C3 | 120.0 (2) |
N1—Ag1—Ag1ii | 99.63 (7) | C5—C4—H4 | 120.0 |
N2i—Ag1—Ag1ii | 86.18 (7) | C3—C4—H4 | 120.0 |
O1—Ag1—Ag1ii | 58.52 (7) | N1—C5—C4 | 122.7 (2) |
O2ii—Ag1—Ag1ii | 104.30 (5) | N1—C5—H5 | 118.7 |
O1—Br1—O3 | 104.86 (17) | C4—C5—H5 | 118.7 |
O1—Br1—O2 | 104.90 (17) | N2—C6—C7 | 122.6 (2) |
O3—Br1—O2 | 106.24 (15) | N2—C6—H6 | 118.7 |
Br1—O1—Ag1 | 166.38 (18) | C7—C6—H6 | 118.7 |
H1w1—O1w—H1w2 | 107.1 (17) | C6—C7—C8 | 119.5 (2) |
H2w1—O2w—H2w2 | 105.7 (17) | C6—C7—H7 | 120.3 |
H3w1—O3w—H3w2 | 109.9 (19) | C8—C7—H7 | 120.3 |
C1—N1—C5 | 117.5 (2) | C9—C8—C7 | 117.2 (2) |
C1—N1—Ag1 | 120.05 (18) | C9—C8—C3 | 121.7 (2) |
C5—N1—Ag1 | 122.37 (18) | C7—C8—C3 | 121.1 (2) |
C10—N2—C6 | 118.0 (2) | C10—C9—C8 | 119.7 (3) |
C10—N2—Ag1iii | 121.96 (18) | C10—C9—H9 | 120.1 |
C6—N2—Ag1iii | 119.35 (18) | C8—C9—H9 | 120.1 |
N1—C1—C2 | 122.5 (3) | N2—C10—C9 | 122.9 (3) |
N1—C1—H1 | 118.7 | N2—C10—H10 | 118.5 |
C2—C1—H1 | 118.7 | C9—C10—H10 | 118.5 |
C1—C2—C3 | 119.7 (3) | | |
| | | |
O3—Br1—O1—Ag1 | 76.8 (8) | C8—C3—C4—C5 | −177.8 (2) |
O2—Br1—O1—Ag1 | −34.9 (8) | C1—N1—C5—C4 | −1.2 (4) |
N1—Ag1—O1—Br1 | 136.6 (7) | Ag1—N1—C5—C4 | 175.5 (2) |
N2i—Ag1—O1—Br1 | −51.2 (7) | C3—C4—C5—N1 | 0.6 (4) |
O2ii—Ag1—O1—Br1 | 48.9 (8) | C10—N2—C6—C7 | −1.6 (4) |
Ag1ii—Ag1—O1—Br1 | 34.2 (7) | Ag1iii—N2—C6—C7 | 169.3 (2) |
O1—Ag1—N1—C1 | −168.7 (2) | N2—C6—C7—C8 | 0.0 (4) |
O2ii—Ag1—N1—C1 | −6.3 (2) | C6—C7—C8—C9 | 1.8 (4) |
Ag1ii—Ag1—N1—C1 | −111.0 (2) | C6—C7—C8—C3 | −176.0 (3) |
O1—Ag1—N1—C5 | 14.7 (2) | C2—C3—C8—C9 | −147.8 (3) |
O2ii—Ag1—N1—C5 | 177.0 (2) | C4—C3—C8—C9 | 30.5 (4) |
Ag1ii—Ag1—N1—C5 | 72.3 (2) | C2—C3—C8—C7 | 30.0 (4) |
C5—N1—C1—C2 | 0.7 (4) | C4—C3—C8—C7 | −151.8 (3) |
Ag1—N1—C1—C2 | −176.1 (2) | C7—C8—C9—C10 | −2.0 (4) |
N1—C1—C2—C3 | 0.4 (4) | C3—C8—C9—C10 | 175.8 (2) |
C1—C2—C3—C4 | −1.0 (4) | C6—N2—C10—C9 | 1.4 (4) |
C1—C2—C3—C8 | 177.4 (3) | Ag1iii—N2—C10—C9 | −169.3 (2) |
C2—C3—C4—C5 | 0.5 (4) | C8—C9—C10—N2 | 0.5 (4) |
Symmetry codes: (i) x+1/2, −y+5/2, z−1/2; (ii) −x, −y+2, −z+1; (iii) x−1/2, −y+5/2, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O2 | 0.86 (1) | 2.12 (3) | 2.927 (5) | 155 (6) |
O1w—H1w1···O3w | 0.86 (1) | 2.46 (6) | 2.894 (5) | 112 (5) |
O2w—H2w1···O2wiv | 0.87 (1) | 2.18 (5) | 2.76 (1) | 124 (5) |
O2w—H2w2···O3v | 0.86 (1) | 2.13 (4) | 2.853 (5) | 141 (5) |
Symmetry codes: (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+1. |