Poly[aqua­(μ₃-3,5-dinitro­salicylato)calcium(II)]

In the title coordination polymer, [Ca(C₇H₂N₂O₇)(H₂O)]_n, the Ca^II 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.

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

No syntax errors found



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

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Computing details

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)]

Crystal data

[Ca(C7H2N2O7)(H2O)]	F(000) = 576
Mr = 284.20	Dx = 1.914 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5209 reflections
a = 12.6381 (4) Å	θ = 3.4–27.7°
b = 6.6650 (3) Å	µ = 0.68 mm^−1
c = 12.4126 (5) Å	T = 293 K
β = 109.391 (2)°	Prism, yellow
V = 986.24 (7) Å^3	0.25 × 0.22 × 0.20 mm
Z = 4

Data collection

Bruker APEX-II area-detector diffractometer	2301 independent reflections
Radiation source: fine-focus sealed tube	2059 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 27.7°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→16
Tmin = 0.849, Tmax = 0.876	k = −8→6
9924 measured reflections	l = −16→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.127	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0756P)^2 + 1.0265P] where P = (Fo^2 + 2Fc^2)/3
2301 reflections	(Δ/σ)max < 0.001
163 parameters	Δρmax = 0.76 e Å^−3
3 restraints	Δρmin = −0.85 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	0.68077 (17)	0.2218 (3)	0.05141 (16)	0.0168 (4)
C2	0.68435 (18)	0.4079 (3)	0.11161 (17)	0.0191 (4)
C3	0.7769 (2)	0.5314 (4)	0.1373 (2)	0.0259 (5)
H3	0.7764	0.6547	0.1722	0.031*
C4	0.8710 (2)	0.4721 (4)	0.1111 (2)	0.0282 (5)
C5	0.87454 (18)	0.2952 (4)	0.0560 (2)	0.0268 (5)
H5	0.9392	0.2554	0.0419	0.032*
C6	0.77878 (18)	0.1775 (3)	0.02212 (18)	0.0212 (4)
C7	0.78239 (18)	−0.0009 (3)	−0.04318 (19)	0.0197 (4)
Ca1	0.48312 (3)	0.01488 (6)	−0.16040 (3)	0.01721 (16)
H1W	0.2757	0.1268	−0.3348	0.030*
H2W	0.2401	−0.0439	−0.3137	0.030*
N1	0.9703 (2)	0.5985 (4)	0.1469 (2)	0.0412 (6)
N2	0.58967 (19)	0.4676 (3)	0.15310 (19)	0.0291 (5)
O1	0.59571 (12)	0.1051 (2)	0.02700 (13)	0.0207 (3)
O2	0.69375 (16)	−0.0846 (3)	−0.09917 (17)	0.0377 (5)
O3	0.87192 (19)	−0.0631 (5)	−0.0444 (3)	0.0656 (8)
O4	0.9629 (2)	0.7628 (5)	0.1873 (3)	0.0755 (9)
O5	1.05667 (18)	0.5356 (4)	0.1346 (2)	0.0538 (6)
O6	0.56667 (16)	0.6478 (3)	0.15572 (17)	0.0331 (4)
O7	0.54175 (14)	0.3319 (2)	0.19177 (15)	0.0262 (4)
O1W	0.29631 (16)	0.0249 (3)	−0.29719 (19)	0.0389 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0183 (9)	0.0168 (9)	0.0154 (9)	−0.0003 (8)	0.0059 (7)	0.0015 (7)
C2	0.0233 (10)	0.0154 (10)	0.0198 (10)	−0.0018 (8)	0.0088 (8)	0.0003 (8)
C3	0.0314 (12)	0.0223 (11)	0.0257 (12)	−0.0082 (9)	0.0116 (10)	−0.0047 (9)
C4	0.0231 (12)	0.0348 (14)	0.0264 (12)	−0.0120 (9)	0.0080 (9)	−0.0025 (10)
C5	0.0197 (10)	0.0368 (13)	0.0256 (11)	−0.0016 (9)	0.0098 (8)	0.0015 (10)
C6	0.0222 (10)	0.0214 (11)	0.0216 (10)	0.0005 (8)	0.0094 (8)	−0.0022 (8)
C7	0.0188 (10)	0.0212 (11)	0.0213 (10)	0.0043 (8)	0.0098 (8)	−0.0050 (8)
Ca1	0.0211 (3)	0.0138 (2)	0.0186 (3)	−0.00120 (14)	0.00912 (18)	0.00004 (14)
N1	0.0324 (12)	0.0569 (16)	0.0329 (12)	−0.0234 (12)	0.0091 (9)	−0.0064 (11)
N2	0.0332 (11)	0.0251 (11)	0.0295 (11)	0.0005 (8)	0.0112 (9)	−0.0040 (8)
O1	0.0223 (7)	0.0208 (8)	0.0217 (7)	−0.0071 (6)	0.0110 (6)	−0.0049 (6)
O2	0.0330 (9)	0.0374 (11)	0.0413 (10)	0.0024 (8)	0.0104 (8)	−0.0194 (9)
O3	0.0350 (11)	0.0677 (17)	0.099 (2)	0.0058 (11)	0.0286 (13)	−0.0403 (16)
O4	0.0654 (17)	0.0681 (18)	0.097 (2)	−0.0457 (15)	0.0323 (16)	−0.0427 (17)
O5	0.0249 (10)	0.0832 (18)	0.0528 (14)	−0.0194 (10)	0.0122 (9)	0.0009 (12)
O6	0.0386 (10)	0.0152 (8)	0.0463 (11)	0.0056 (7)	0.0153 (8)	−0.0039 (7)
O7	0.0363 (9)	0.0177 (8)	0.0345 (9)	−0.0022 (7)	0.0250 (7)	−0.0034 (6)
O1W	0.0301 (10)	0.0306 (11)	0.0431 (12)	−0.0077 (8)	−0.0050 (9)	0.0124 (9)

Geometric parameters (Å, º)

C1—O1	1.279 (3)	Ca1—O1W	2.408 (2)
C1—C6	1.433 (3)	Ca1—O7^iii	2.4210 (15)
C1—C2	1.441 (3)	Ca1—O2	2.5999 (19)
C2—C3	1.378 (3)	Ca1—O6^iii	3.017 (2)
C2—N2	1.505 (3)	Ca1—Ca1^i	3.8665 (8)
C3—C4	1.390 (3)	Ca1—Ca1^iv	4.1067 (5)
C3—H3	0.9300	N1—O4	1.221 (4)
C4—C5	1.371 (4)	N1—O5	1.225 (4)
C4—N1	1.453 (3)	N2—O6	1.239 (3)
C5—C6	1.385 (3)	N2—O7	1.268 (3)
C5—H5	0.9300	O1—Ca1^i	2.3386 (14)
C6—C7	1.448 (3)	O6—Ca1^ii	2.3407 (17)
C7—O3	1.210 (3)	O6—Ca1^v	3.017 (2)
C7—O2	1.238 (3)	O7—Ca1^i	2.3476 (16)
Ca1—O1^i	2.3386 (14)	O7—Ca1^v	2.4210 (15)
Ca1—O6^ii	2.3407 (17)	O1W—H1W	0.8161
Ca1—O7^i	2.3476 (16)	O1W—H2W	0.8121
Ca1—O1	2.3662 (15)
O1—C1—C6	122.96 (19)	O7^i—Ca1—N2^iii	88.88 (6)
O1—C1—C2	121.69 (18)	O1—Ca1—N2^iii	117.69 (6)
C6—C1—C2	115.34 (18)	O1W—Ca1—N2^iii	92.32 (7)
C3—C2—C1	120.81 (19)	O1W—Ca1—C1^i	72.21 (6)
C3—C2—N2	118.25 (19)	O7^iii—Ca1—C1^i	157.22 (6)
C1—C2—N2	120.88 (18)	O2—Ca1—C1^i	119.27 (6)
C2—C3—C4	120.1 (2)	O6^iii—Ca1—C1^i	125.07 (5)
C2—C3—H3	119.9	N2^iii—Ca1—C1^i	147.50 (6)
C4—C3—H3	119.9	O1^i—Ca1—Ca1^i	34.97 (4)
C5—C4—C3	122.2 (2)	O6^ii—Ca1—Ca1^i	87.84 (5)
C5—C4—N1	118.9 (2)	O7^i—Ca1—Ca1^i	94.77 (4)
C3—C4—N1	118.9 (2)	O1—Ca1—Ca1^i	34.50 (3)
C4—C5—C6	117.9 (2)	O1W—Ca1—Ca1^i	118.34 (6)
C4—C5—H5	121.0	O7^iii—Ca1—Ca1^i	147.71 (5)
C6—C5—H5	121.0	O2—Ca1—Ca1^i	86.20 (5)
C5—C6—C1	123.2 (2)	O6^iii—Ca1—Ca1^i	144.50 (4)
C5—C6—C7	116.62 (19)	N2^iii—Ca1—Ca1^i	149.34 (5)
C1—C6—C7	120.12 (19)	C1^i—Ca1—Ca1^i	53.94 (4)
O3—C7—O2	121.0 (2)	O1^i—Ca1—Ca1^iv	104.56 (4)
O3—C7—C6	119.5 (2)	O6^ii—Ca1—Ca1^iv	150.46 (5)
O2—C7—C6	119.56 (19)	O7^i—Ca1—Ca1^iv	31.07 (4)
O1^i—Ca1—O6^ii	97.45 (6)	O1—Ca1—Ca1^iv	127.01 (4)
O1^i—Ca1—O7^i	73.49 (5)	O1W—Ca1—Ca1^iv	83.94 (6)
O6^ii—Ca1—O7^i	158.05 (7)	O7^iii—Ca1—Ca1^iv	79.56 (4)
O1^i—Ca1—O1	69.47 (6)	O2—Ca1—Ca1^iv	70.79 (4)
O6^ii—Ca1—O1	79.07 (6)	O6^iii—Ca1—Ca1^iv	34.23 (3)
O7^i—Ca1—O1	114.64 (6)	N2^iii—Ca1—Ca1^iv	57.81 (4)
O1^i—Ca1—O1W	87.73 (7)	C1^i—Ca1—Ca1^iv	91.54 (4)
O6^ii—Ca1—O1W	77.42 (7)	Ca1^i—Ca1—Ca1^iv	121.358 (15)
O7^i—Ca1—O1W	82.21 (7)	O4—N1—O5	123.4 (2)
O1—Ca1—O1W	144.57 (7)	O4—N1—C4	118.0 (2)
O1^i—Ca1—O7^iii	172.04 (6)	O5—N1—C4	118.6 (3)
O6^ii—Ca1—O7^iii	76.47 (6)	O6—N2—O7	122.4 (2)
O7^i—Ca1—O7^iii	110.33 (4)	O6—N2—C2	119.0 (2)
O1—Ca1—O7^iii	113.73 (6)	O7—N2—C2	118.38 (19)
O1W—Ca1—O7^iii	85.93 (7)	O6—N2—Ca1^v	77.04 (13)
O1^i—Ca1—O2	109.96 (6)	O7—N2—Ca1^v	49.58 (10)
O6^ii—Ca1—O2	119.69 (7)	C2—N2—Ca1^v	150.90 (15)
O7^i—Ca1—O2	82.25 (6)	C1—O1—Ca1^i	124.21 (12)
O1—Ca1—O2	63.53 (5)	C1—O1—Ca1	124.83 (12)
O1W—Ca1—O2	151.90 (7)	Ca1^i—O1—Ca1	110.53 (6)
O7^iii—Ca1—O2	77.75 (6)	C7—O2—Ca1	134.20 (15)
O1^i—Ca1—O6^iii	138.70 (5)	N2—O6—Ca1^ii	178.00 (17)
O6^ii—Ca1—O6^iii	121.90 (5)	N2—O6—Ca1^v	79.37 (14)
O7^i—Ca1—O6^iii	65.28 (5)	Ca1^ii—O6—Ca1^v	99.32 (6)
O1—Ca1—O6^iii	126.00 (5)	N2—O7—Ca1^i	133.92 (13)
O1W—Ca1—O6^iii	89.08 (7)	N2—O7—Ca1^v	106.92 (13)
O7^iii—Ca1—O6^iii	46.06 (5)	Ca1^i—O7—Ca1^v	118.89 (6)
O2—Ca1—O6^iii	63.12 (6)	Ca1—O1W—H1W	118.6
O1^i—Ca1—N2^iii	162.20 (6)	Ca1—O1W—H2W	137.1
O6^ii—Ca1—N2^iii	99.93 (6)	H1W—O1W—H2W	103.8

Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z; (iii) x, −y+1/2, z−1/2; (iv) −x+1, y−1/2, −z−1/2; (v) x, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···O5^vi	0.81	2.19	2.889 (3)	144
O1W—H1W···O2^vii	0.82	2.18	2.924 (3)	153

Symmetry codes: (vi) x−1, −y+1/2, z−1/2; (vii) −x+1, y+1/2, −z−1/2.