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In the title coordination polymer, [Ca(C7H2N2O7)(H2O)]n, the CaII atom is seven-coordinate by six O atoms from four 3,5-dinitro­salicylatate ligands and one water mol­ecule, and displays a distorted penta­gonal–bipyramidal geometry. Centrosymmetrically related dinuclear calcium units with a Ca...Ca separation of 3.8665 (8)Å form layers which are self-assembled into a three-dimensional network by inter­molecular O—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055553/rz2102sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055553/rz2102Isup2.hkl
Contains datablock I

CCDC reference: 636780

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.040
  • wR factor = 0.127
  • Data-to-parameter ratio = 14.1

checkCIF/PLATON results

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Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.65 Ratio
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C7 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.35 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker,1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Poly[aqua(µ3-3,5-dinitrosalicylato)calcium(II)] top
Crystal data top
[Ca(C7H2N2O7)(H2O)]F(000) = 576
Mr = 284.20Dx = 1.914 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5209 reflections
a = 12.6381 (4) Åθ = 3.4–27.7°
b = 6.6650 (3) ŵ = 0.68 mm1
c = 12.4126 (5) ÅT = 293 K
β = 109.391 (2)°Prism, yellow
V = 986.24 (7) Å30.25 × 0.22 × 0.20 mm
Z = 4
Data collection top
Bruker APEX-II area-detector
diffractometer
2301 independent reflections
Radiation source: fine-focus sealed tube2059 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 27.7°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1616
Tmin = 0.849, Tmax = 0.876k = 86
9924 measured reflectionsl = 1616
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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0756P)2 + 1.0265P]
where P = (Fo2 + 2Fc2)/3
2301 reflections(Δ/σ)max < 0.001
163 parametersΔρmax = 0.76 e Å3
3 restraintsΔρmin = 0.85 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
C10.68077 (17)0.2218 (3)0.05141 (16)0.0168 (4)
C20.68435 (18)0.4079 (3)0.11161 (17)0.0191 (4)
C30.7769 (2)0.5314 (4)0.1373 (2)0.0259 (5)
H30.77640.65470.17220.031*
C40.8710 (2)0.4721 (4)0.1111 (2)0.0282 (5)
C50.87454 (18)0.2952 (4)0.0560 (2)0.0268 (5)
H50.93920.25540.04190.032*
C60.77878 (18)0.1775 (3)0.02212 (18)0.0212 (4)
C70.78239 (18)0.0009 (3)0.04318 (19)0.0197 (4)
Ca10.48312 (3)0.01488 (6)0.16040 (3)0.01721 (16)
H1W0.27570.12680.33480.030*
H2W0.24010.04390.31370.030*
N10.9703 (2)0.5985 (4)0.1469 (2)0.0412 (6)
N20.58967 (19)0.4676 (3)0.15310 (19)0.0291 (5)
O10.59571 (12)0.1051 (2)0.02700 (13)0.0207 (3)
O20.69375 (16)0.0846 (3)0.09917 (17)0.0377 (5)
O30.87192 (19)0.0631 (5)0.0444 (3)0.0656 (8)
O40.9629 (2)0.7628 (5)0.1873 (3)0.0755 (9)
O51.05667 (18)0.5356 (4)0.1346 (2)0.0538 (6)
O60.56667 (16)0.6478 (3)0.15572 (17)0.0331 (4)
O70.54175 (14)0.3319 (2)0.19177 (15)0.0262 (4)
O1W0.29631 (16)0.0249 (3)0.29719 (19)0.0389 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0183 (9)0.0168 (9)0.0154 (9)0.0003 (8)0.0059 (7)0.0015 (7)
C20.0233 (10)0.0154 (10)0.0198 (10)0.0018 (8)0.0088 (8)0.0003 (8)
C30.0314 (12)0.0223 (11)0.0257 (12)0.0082 (9)0.0116 (10)0.0047 (9)
C40.0231 (12)0.0348 (14)0.0264 (12)0.0120 (9)0.0080 (9)0.0025 (10)
C50.0197 (10)0.0368 (13)0.0256 (11)0.0016 (9)0.0098 (8)0.0015 (10)
C60.0222 (10)0.0214 (11)0.0216 (10)0.0005 (8)0.0094 (8)0.0022 (8)
C70.0188 (10)0.0212 (11)0.0213 (10)0.0043 (8)0.0098 (8)0.0050 (8)
Ca10.0211 (3)0.0138 (2)0.0186 (3)0.00120 (14)0.00912 (18)0.00004 (14)
N10.0324 (12)0.0569 (16)0.0329 (12)0.0234 (12)0.0091 (9)0.0064 (11)
N20.0332 (11)0.0251 (11)0.0295 (11)0.0005 (8)0.0112 (9)0.0040 (8)
O10.0223 (7)0.0208 (8)0.0217 (7)0.0071 (6)0.0110 (6)0.0049 (6)
O20.0330 (9)0.0374 (11)0.0413 (10)0.0024 (8)0.0104 (8)0.0194 (9)
O30.0350 (11)0.0677 (17)0.099 (2)0.0058 (11)0.0286 (13)0.0403 (16)
O40.0654 (17)0.0681 (18)0.097 (2)0.0457 (15)0.0323 (16)0.0427 (17)
O50.0249 (10)0.0832 (18)0.0528 (14)0.0194 (10)0.0122 (9)0.0009 (12)
O60.0386 (10)0.0152 (8)0.0463 (11)0.0056 (7)0.0153 (8)0.0039 (7)
O70.0363 (9)0.0177 (8)0.0345 (9)0.0022 (7)0.0250 (7)0.0034 (6)
O1W0.0301 (10)0.0306 (11)0.0431 (12)0.0077 (8)0.0050 (9)0.0124 (9)
Geometric parameters (Å, º) top
C1—O11.279 (3)Ca1—O1W2.408 (2)
C1—C61.433 (3)Ca1—O7iii2.4210 (15)
C1—C21.441 (3)Ca1—O22.5999 (19)
C2—C31.378 (3)Ca1—O6iii3.017 (2)
C2—N21.505 (3)Ca1—Ca1i3.8665 (8)
C3—C41.390 (3)Ca1—Ca1iv4.1067 (5)
C3—H30.9300N1—O41.221 (4)
C4—C51.371 (4)N1—O51.225 (4)
C4—N11.453 (3)N2—O61.239 (3)
C5—C61.385 (3)N2—O71.268 (3)
C5—H50.9300O1—Ca1i2.3386 (14)
C6—C71.448 (3)O6—Ca1ii2.3407 (17)
C7—O31.210 (3)O6—Ca1v3.017 (2)
C7—O21.238 (3)O7—Ca1i2.3476 (16)
Ca1—O1i2.3386 (14)O7—Ca1v2.4210 (15)
Ca1—O6ii2.3407 (17)O1W—H1W0.8161
Ca1—O7i2.3476 (16)O1W—H2W0.8121
Ca1—O12.3662 (15)
O1—C1—C6122.96 (19)O7i—Ca1—N2iii88.88 (6)
O1—C1—C2121.69 (18)O1—Ca1—N2iii117.69 (6)
C6—C1—C2115.34 (18)O1W—Ca1—N2iii92.32 (7)
C3—C2—C1120.81 (19)O1W—Ca1—C1i72.21 (6)
C3—C2—N2118.25 (19)O7iii—Ca1—C1i157.22 (6)
C1—C2—N2120.88 (18)O2—Ca1—C1i119.27 (6)
C2—C3—C4120.1 (2)O6iii—Ca1—C1i125.07 (5)
C2—C3—H3119.9N2iii—Ca1—C1i147.50 (6)
C4—C3—H3119.9O1i—Ca1—Ca1i34.97 (4)
C5—C4—C3122.2 (2)O6ii—Ca1—Ca1i87.84 (5)
C5—C4—N1118.9 (2)O7i—Ca1—Ca1i94.77 (4)
C3—C4—N1118.9 (2)O1—Ca1—Ca1i34.50 (3)
C4—C5—C6117.9 (2)O1W—Ca1—Ca1i118.34 (6)
C4—C5—H5121.0O7iii—Ca1—Ca1i147.71 (5)
C6—C5—H5121.0O2—Ca1—Ca1i86.20 (5)
C5—C6—C1123.2 (2)O6iii—Ca1—Ca1i144.50 (4)
C5—C6—C7116.62 (19)N2iii—Ca1—Ca1i149.34 (5)
C1—C6—C7120.12 (19)C1i—Ca1—Ca1i53.94 (4)
O3—C7—O2121.0 (2)O1i—Ca1—Ca1iv104.56 (4)
O3—C7—C6119.5 (2)O6ii—Ca1—Ca1iv150.46 (5)
O2—C7—C6119.56 (19)O7i—Ca1—Ca1iv31.07 (4)
O1i—Ca1—O6ii97.45 (6)O1—Ca1—Ca1iv127.01 (4)
O1i—Ca1—O7i73.49 (5)O1W—Ca1—Ca1iv83.94 (6)
O6ii—Ca1—O7i158.05 (7)O7iii—Ca1—Ca1iv79.56 (4)
O1i—Ca1—O169.47 (6)O2—Ca1—Ca1iv70.79 (4)
O6ii—Ca1—O179.07 (6)O6iii—Ca1—Ca1iv34.23 (3)
O7i—Ca1—O1114.64 (6)N2iii—Ca1—Ca1iv57.81 (4)
O1i—Ca1—O1W87.73 (7)C1i—Ca1—Ca1iv91.54 (4)
O6ii—Ca1—O1W77.42 (7)Ca1i—Ca1—Ca1iv121.358 (15)
O7i—Ca1—O1W82.21 (7)O4—N1—O5123.4 (2)
O1—Ca1—O1W144.57 (7)O4—N1—C4118.0 (2)
O1i—Ca1—O7iii172.04 (6)O5—N1—C4118.6 (3)
O6ii—Ca1—O7iii76.47 (6)O6—N2—O7122.4 (2)
O7i—Ca1—O7iii110.33 (4)O6—N2—C2119.0 (2)
O1—Ca1—O7iii113.73 (6)O7—N2—C2118.38 (19)
O1W—Ca1—O7iii85.93 (7)O6—N2—Ca1v77.04 (13)
O1i—Ca1—O2109.96 (6)O7—N2—Ca1v49.58 (10)
O6ii—Ca1—O2119.69 (7)C2—N2—Ca1v150.90 (15)
O7i—Ca1—O282.25 (6)C1—O1—Ca1i124.21 (12)
O1—Ca1—O263.53 (5)C1—O1—Ca1124.83 (12)
O1W—Ca1—O2151.90 (7)Ca1i—O1—Ca1110.53 (6)
O7iii—Ca1—O277.75 (6)C7—O2—Ca1134.20 (15)
O1i—Ca1—O6iii138.70 (5)N2—O6—Ca1ii178.00 (17)
O6ii—Ca1—O6iii121.90 (5)N2—O6—Ca1v79.37 (14)
O7i—Ca1—O6iii65.28 (5)Ca1ii—O6—Ca1v99.32 (6)
O1—Ca1—O6iii126.00 (5)N2—O7—Ca1i133.92 (13)
O1W—Ca1—O6iii89.08 (7)N2—O7—Ca1v106.92 (13)
O7iii—Ca1—O6iii46.06 (5)Ca1i—O7—Ca1v118.89 (6)
O2—Ca1—O6iii63.12 (6)Ca1—O1W—H1W118.6
O1i—Ca1—N2iii162.20 (6)Ca1—O1W—H2W137.1
O6ii—Ca1—N2iii99.93 (6)H1W—O1W—H2W103.8
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1, z; (iii) x, y+1/2, z1/2; (iv) x+1, y1/2, z1/2; (v) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H2W···O5vi0.812.192.889 (3)144
O1W—H1W···O2vii0.822.182.924 (3)153
Symmetry codes: (vi) x1, y+1/2, z1/2; (vii) x+1, y+1/2, z1/2.
 

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