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In the title complex, {[CaMn(C4H4O5)2(H2O)6]·2H2O}n, the CaII and MnII ions are bridged by oxydiacetate (ODA) dianions to form zigzag polymeric chains. The CaII ion is located at a twofold axis and is coordinated by two tridentate ODA and two water mol­ecules with a distorted tetra­gonal antiprism coordination geometry. The MnII ion is located at another twofold axis, and assumes a distorted octa­hedral coordination geometry formed by four water mol­ecules and two carboxyl O atoms from monodentate ODA dianions also chelating to the neighboring CaII atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502622X/hb6250sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680502622X/hb6250Isup2.hkl
Contains datablock I

CCDC reference: 283920

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.039
  • wR factor = 0.154
  • Data-to-parameter ratio = 18.6

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 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 2 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

catena-Poly[[[diaquacalcium(II)]-µ-oxydiacetato-[tetraaquamanganese(II)]- µ-oxydiacetato] dihydrate] top
Crystal data top
[CaMn(C4H4O5)2(H2O)6]·2H2OF(000) = 1044
Mr = 503.29Dx = 1.739 Mg m3
Dm = 1.741 Mg m3
Dm measured by flotation in CHBr3/CCl4
Orthorhombic, PccnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2acCell parameters from 3866 reflections
a = 9.9572 (18) Åθ = 3.0–25.0°
b = 12.819 (2) ŵ = 1.04 mm1
c = 15.061 (3) ÅT = 295 K
V = 1922.4 (6) Å3Prism, colorless
Z = 40.40 × 0.38 × 0.30 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2379 independent reflections
Radiation source: fine-focus sealed tube1341 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
Detector resolution: 10.00 pixels mm-1θmax = 28.3°, θmin = 2.6°
ω scansh = 1213
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1717
Tmin = 0.678, Tmax = 0.736l = 2010
11775 measured reflections
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)] = 0.039Hydrogen site location: difmap (O-H) and geom (others)
wR(F2) = 0.154H-atom parameters constrained
S = 0.87 w = 1/[σ2(Fo2) + (0.0832P)2 + 3.6036P]
where P = (Fo2 + 2Fc2)/3
2379 reflections(Δ/σ)max = 0.001
128 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = 0.53 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
Mn0.25000.25000.67634 (5)0.0305 (2)
Ca0.75000.25000.52913 (6)0.0251 (2)
O10.8710 (2)0.3509 (2)0.41892 (17)0.0374 (6)
O20.8712 (2)0.4164 (2)0.28151 (17)0.0368 (6)
O30.6171 (2)0.3791 (2)0.44189 (16)0.0329 (6)
O40.5280 (3)0.2846 (2)0.58175 (18)0.0428 (7)
O50.3218 (2)0.3453 (2)0.56620 (17)0.0396 (7)
O60.7044 (3)0.1081 (2)0.63016 (18)0.0394 (6)
H6A0.76050.08610.66550.059*
H6B0.67850.05100.60680.059*
O70.1367 (3)0.1533 (2)0.76857 (19)0.0508 (8)
H7A0.16330.14940.82400.076*
H7B0.04160.13810.77050.076*
O80.0887 (3)0.3662 (2)0.6947 (2)0.0487 (8)
H8A0.10160.43610.70400.073*
H8B0.01440.35660.67080.073*
O1W0.1402 (3)0.4153 (2)0.44165 (18)0.0439 (7)
H1A0.05720.39570.44650.066*
H1B0.18420.39630.48520.066*
C10.8143 (3)0.3885 (3)0.3526 (2)0.0286 (7)
C20.6640 (3)0.4021 (3)0.3549 (2)0.0326 (8)
H2A0.64060.47320.33920.039*
H2B0.62220.35550.31230.039*
C30.4751 (3)0.3764 (3)0.4494 (2)0.0323 (8)
H3A0.43720.33280.40310.039*
H3B0.43850.44620.44330.039*
C40.4410 (3)0.3324 (3)0.5396 (2)0.0291 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0346 (4)0.0326 (4)0.0243 (4)0.0024 (3)0.0000.000
Ca0.0237 (5)0.0308 (5)0.0208 (5)0.0006 (4)0.0000.000
O10.0272 (13)0.0518 (16)0.0331 (14)0.0024 (11)0.0007 (11)0.0105 (13)
O20.0334 (14)0.0481 (15)0.0289 (14)0.0014 (12)0.0069 (11)0.0067 (12)
O30.0261 (12)0.0467 (15)0.0260 (13)0.0005 (11)0.0054 (10)0.0091 (11)
O40.0332 (14)0.0598 (17)0.0355 (15)0.0072 (13)0.0054 (12)0.0153 (13)
O50.0306 (14)0.0525 (16)0.0358 (15)0.0017 (12)0.0082 (12)0.0088 (13)
O60.0464 (15)0.0392 (14)0.0326 (15)0.0013 (12)0.0044 (13)0.0031 (12)
O70.0420 (16)0.071 (2)0.0393 (16)0.0151 (14)0.0002 (14)0.0147 (15)
O80.0305 (14)0.0478 (16)0.068 (2)0.0015 (12)0.0010 (14)0.0151 (15)
O1W0.0373 (15)0.0563 (18)0.0381 (16)0.0044 (13)0.0026 (13)0.0090 (13)
C10.0324 (18)0.0284 (16)0.0250 (17)0.0002 (15)0.0038 (15)0.0003 (14)
C20.0308 (17)0.043 (2)0.0242 (17)0.0001 (16)0.0022 (15)0.0081 (16)
C30.0241 (16)0.042 (2)0.0312 (19)0.0019 (15)0.0024 (15)0.0050 (16)
C40.0285 (17)0.0300 (17)0.0289 (18)0.0027 (14)0.0035 (15)0.0015 (15)
Geometric parameters (Å, º) top
Mn—O5i2.181 (3)O3—C21.422 (4)
Mn—O52.181 (3)O4—C41.236 (4)
Mn—O7i2.177 (3)O5—C41.264 (4)
Mn—O72.177 (3)O6—H6A0.8214
Mn—O82.207 (3)O6—H6B0.8520
Mn—O8i2.207 (3)O7—H7A0.8764
Ca—O1ii2.425 (3)O7—H7B0.9675
Ca—O12.425 (3)O8—H8A0.9164
Ca—O3ii2.493 (2)O8—H8B0.8324
Ca—O32.493 (2)O1W—H1A0.8669
Ca—O4ii2.390 (3)O1W—H1B0.8254
Ca—O42.390 (3)C1—C21.508 (5)
Ca—O6ii2.415 (3)C2—H2A0.9700
Ca—O62.415 (3)C2—H2B0.9700
O1—C11.244 (4)C3—C41.510 (5)
O2—C11.263 (4)C3—H3A0.9700
O3—C31.419 (4)C3—H3B0.9700
O7i—Mn—O7100.71 (16)O6—Ca—O3137.09 (8)
O7i—Mn—O5i166.99 (10)O1ii—Ca—O374.30 (9)
O7—Mn—O5i89.79 (11)O1—Ca—O363.19 (8)
O7i—Mn—O589.79 (11)O3ii—Ca—O3116.38 (12)
O7—Mn—O5166.99 (10)C1—O1—Ca122.1 (2)
O5i—Mn—O580.95 (15)C3—O3—C2113.9 (3)
O7i—Mn—O884.98 (11)C3—O3—Ca118.1 (2)
O7—Mn—O885.84 (12)C2—O3—Ca116.7 (2)
O5i—Mn—O8103.60 (11)C4—O4—Ca124.7 (2)
O5—Mn—O887.46 (11)C4—O5—Mn118.4 (2)
O7i—Mn—O8i85.84 (12)Ca—O6—H6A122.6
O7—Mn—O8i84.98 (11)Ca—O6—H6B116.3
O5i—Mn—O8i87.46 (11)H6A—O6—H6B100.3
O5—Mn—O8i103.60 (11)Mn—O7—H7A118.9
O8—Mn—O8i165.58 (17)Mn—O7—H7B129.9
O4ii—Ca—O4141.27 (14)H7A—O7—H7B104.8
O4ii—Ca—O6ii75.93 (9)Mn—O8—H8A125.3
O4—Ca—O6ii79.93 (10)Mn—O8—H8B119.5
O4ii—Ca—O679.93 (10)H8A—O8—H8B109.5
O4—Ca—O675.93 (9)H1A—O1W—H1B110.7
O6ii—Ca—O6101.88 (13)O1—C1—O2126.0 (3)
O4ii—Ca—O1ii126.00 (9)O1—C1—C2118.5 (3)
O4—Ca—O1ii82.31 (10)O2—C1—C2115.6 (3)
O6ii—Ca—O1ii157.90 (9)O3—C2—C1108.8 (3)
O6—Ca—O1ii86.35 (9)O3—C2—H2A109.9
O4ii—Ca—O182.31 (10)C1—C2—H2A109.9
O4—Ca—O1126.00 (9)O3—C2—H2B109.9
O6ii—Ca—O186.35 (9)C1—C2—H2B109.9
O6—Ca—O1157.90 (9)H2A—C2—H2B108.3
O1ii—Ca—O193.59 (13)O3—C3—C4107.7 (3)
O4ii—Ca—O3ii63.95 (8)O3—C3—H3A110.2
O4—Ca—O3ii142.07 (9)C4—C3—H3A110.2
O6ii—Ca—O3ii137.09 (8)O3—C3—H3B110.2
O6—Ca—O3ii86.09 (9)C4—C3—H3B110.2
O1ii—Ca—O3ii63.19 (8)H3A—C3—H3B108.5
O1—Ca—O3ii74.30 (9)O4—C4—O5124.1 (3)
O4ii—Ca—O3142.07 (9)O4—C4—C3119.3 (3)
O4—Ca—O363.95 (8)O5—C4—C3116.6 (3)
O6ii—Ca—O386.09 (9)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+3/2, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1A···O1iii0.871.982.826 (4)163
O1W—H1B···O50.831.952.756 (4)166
O6—H6A···O2iv0.822.072.838 (4)156
O6—H6B···O1Wv0.851.922.772 (4)173
O7—H7A···O1Wiv0.881.972.751 (4)148
O7—H7B···O2vi0.971.842.797 (4)169
O8—H8A···O2vii0.921.922.838 (4)178
O8—H8B···O4i0.832.292.825 (4)122
O8—H8B···O6i0.832.313.094 (4)158
Symmetry codes: (i) x+1/2, y+1/2, z; (iii) x1, y, z; (iv) x, y+1/2, z+1/2; (v) x+1/2, y1/2, z+1; (vi) x1, y+1/2, z+1/2; (vii) x+1, y+1, z+1.
 

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