Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680502622X/hb6250sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680502622X/hb6250Isup2.hkl |
CCDC reference: 283920
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- R factor = 0.039
- wR factor = 0.154
- Data-to-parameter ratio = 18.6
checkCIF/PLATON results
No syntax errors found
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
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).
[CaMn(C4H4O5)2(H2O)6]·2H2O | F(000) = 1044 |
Mr = 503.29 | Dx = 1.739 Mg m−3 Dm = 1.741 Mg m−3 Dm measured by flotation in CHBr3/CCl4 |
Orthorhombic, Pccn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ab 2ac | Cell parameters from 3866 reflections |
a = 9.9572 (18) Å | θ = 3.0–25.0° |
b = 12.819 (2) Å | µ = 1.04 mm−1 |
c = 15.061 (3) Å | T = 295 K |
V = 1922.4 (6) Å3 | Prism, colorless |
Z = 4 | 0.40 × 0.38 × 0.30 mm |
Rigaku R-AXIS RAPID diffractometer | 2379 independent reflections |
Radiation source: fine-focus sealed tube | 1341 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 10.00 pixels mm-1 | θmax = 28.3°, θmin = 2.6° |
ω scans | h = −12→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −17→17 |
Tmin = 0.678, Tmax = 0.736 | l = −20→10 |
11775 measured reflections |
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)] = 0.039 | Hydrogen site location: difmap (O-H) and geom (others) |
wR(F2) = 0.154 | H-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 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.53 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Mn | 0.2500 | 0.2500 | 0.67634 (5) | 0.0305 (2) | |
Ca | 0.7500 | 0.2500 | 0.52913 (6) | 0.0251 (2) | |
O1 | 0.8710 (2) | 0.3509 (2) | 0.41892 (17) | 0.0374 (6) | |
O2 | 0.8712 (2) | 0.4164 (2) | 0.28151 (17) | 0.0368 (6) | |
O3 | 0.6171 (2) | 0.3791 (2) | 0.44189 (16) | 0.0329 (6) | |
O4 | 0.5280 (3) | 0.2846 (2) | 0.58175 (18) | 0.0428 (7) | |
O5 | 0.3218 (2) | 0.3453 (2) | 0.56620 (17) | 0.0396 (7) | |
O6 | 0.7044 (3) | 0.1081 (2) | 0.63016 (18) | 0.0394 (6) | |
H6A | 0.7605 | 0.0861 | 0.6655 | 0.059* | |
H6B | 0.6785 | 0.0510 | 0.6068 | 0.059* | |
O7 | 0.1367 (3) | 0.1533 (2) | 0.76857 (19) | 0.0508 (8) | |
H7A | 0.1633 | 0.1494 | 0.8240 | 0.076* | |
H7B | 0.0416 | 0.1381 | 0.7705 | 0.076* | |
O8 | 0.0887 (3) | 0.3662 (2) | 0.6947 (2) | 0.0487 (8) | |
H8A | 0.1016 | 0.4361 | 0.7040 | 0.073* | |
H8B | 0.0144 | 0.3566 | 0.6708 | 0.073* | |
O1W | 0.1402 (3) | 0.4153 (2) | 0.44165 (18) | 0.0439 (7) | |
H1A | 0.0572 | 0.3957 | 0.4465 | 0.066* | |
H1B | 0.1842 | 0.3963 | 0.4852 | 0.066* | |
C1 | 0.8143 (3) | 0.3885 (3) | 0.3526 (2) | 0.0286 (7) | |
C2 | 0.6640 (3) | 0.4021 (3) | 0.3549 (2) | 0.0326 (8) | |
H2A | 0.6406 | 0.4732 | 0.3392 | 0.039* | |
H2B | 0.6222 | 0.3555 | 0.3123 | 0.039* | |
C3 | 0.4751 (3) | 0.3764 (3) | 0.4494 (2) | 0.0323 (8) | |
H3A | 0.4372 | 0.3328 | 0.4031 | 0.039* | |
H3B | 0.4385 | 0.4462 | 0.4433 | 0.039* | |
C4 | 0.4410 (3) | 0.3324 (3) | 0.5396 (2) | 0.0291 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn | 0.0346 (4) | 0.0326 (4) | 0.0243 (4) | −0.0024 (3) | 0.000 | 0.000 |
Ca | 0.0237 (5) | 0.0308 (5) | 0.0208 (5) | −0.0006 (4) | 0.000 | 0.000 |
O1 | 0.0272 (13) | 0.0518 (16) | 0.0331 (14) | −0.0024 (11) | 0.0007 (11) | 0.0105 (13) |
O2 | 0.0334 (14) | 0.0481 (15) | 0.0289 (14) | 0.0014 (12) | 0.0069 (11) | 0.0067 (12) |
O3 | 0.0261 (12) | 0.0467 (15) | 0.0260 (13) | 0.0005 (11) | 0.0054 (10) | 0.0091 (11) |
O4 | 0.0332 (14) | 0.0598 (17) | 0.0355 (15) | 0.0072 (13) | 0.0054 (12) | 0.0153 (13) |
O5 | 0.0306 (14) | 0.0525 (16) | 0.0358 (15) | 0.0017 (12) | 0.0082 (12) | 0.0088 (13) |
O6 | 0.0464 (15) | 0.0392 (14) | 0.0326 (15) | −0.0013 (12) | −0.0044 (13) | 0.0031 (12) |
O7 | 0.0420 (16) | 0.071 (2) | 0.0393 (16) | −0.0151 (14) | −0.0002 (14) | 0.0147 (15) |
O8 | 0.0305 (14) | 0.0478 (16) | 0.068 (2) | −0.0015 (12) | 0.0010 (14) | −0.0151 (15) |
O1W | 0.0373 (15) | 0.0563 (18) | 0.0381 (16) | −0.0044 (13) | −0.0026 (13) | 0.0090 (13) |
C1 | 0.0324 (18) | 0.0284 (16) | 0.0250 (17) | −0.0002 (15) | 0.0038 (15) | 0.0003 (14) |
C2 | 0.0308 (17) | 0.043 (2) | 0.0242 (17) | 0.0001 (16) | 0.0022 (15) | 0.0081 (16) |
C3 | 0.0241 (16) | 0.042 (2) | 0.0312 (19) | 0.0019 (15) | 0.0024 (15) | 0.0050 (16) |
C4 | 0.0285 (17) | 0.0300 (17) | 0.0289 (18) | −0.0027 (14) | 0.0035 (15) | −0.0015 (15) |
Mn—O5i | 2.181 (3) | O3—C2 | 1.422 (4) |
Mn—O5 | 2.181 (3) | O4—C4 | 1.236 (4) |
Mn—O7i | 2.177 (3) | O5—C4 | 1.264 (4) |
Mn—O7 | 2.177 (3) | O6—H6A | 0.8214 |
Mn—O8 | 2.207 (3) | O6—H6B | 0.8520 |
Mn—O8i | 2.207 (3) | O7—H7A | 0.8764 |
Ca—O1ii | 2.425 (3) | O7—H7B | 0.9675 |
Ca—O1 | 2.425 (3) | O8—H8A | 0.9164 |
Ca—O3ii | 2.493 (2) | O8—H8B | 0.8324 |
Ca—O3 | 2.493 (2) | O1W—H1A | 0.8669 |
Ca—O4ii | 2.390 (3) | O1W—H1B | 0.8254 |
Ca—O4 | 2.390 (3) | C1—C2 | 1.508 (5) |
Ca—O6ii | 2.415 (3) | C2—H2A | 0.9700 |
Ca—O6 | 2.415 (3) | C2—H2B | 0.9700 |
O1—C1 | 1.244 (4) | C3—C4 | 1.510 (5) |
O2—C1 | 1.263 (4) | C3—H3A | 0.9700 |
O3—C3 | 1.419 (4) | C3—H3B | 0.9700 |
O7i—Mn—O7 | 100.71 (16) | O6—Ca—O3 | 137.09 (8) |
O7i—Mn—O5i | 166.99 (10) | O1ii—Ca—O3 | 74.30 (9) |
O7—Mn—O5i | 89.79 (11) | O1—Ca—O3 | 63.19 (8) |
O7i—Mn—O5 | 89.79 (11) | O3ii—Ca—O3 | 116.38 (12) |
O7—Mn—O5 | 166.99 (10) | C1—O1—Ca | 122.1 (2) |
O5i—Mn—O5 | 80.95 (15) | C3—O3—C2 | 113.9 (3) |
O7i—Mn—O8 | 84.98 (11) | C3—O3—Ca | 118.1 (2) |
O7—Mn—O8 | 85.84 (12) | C2—O3—Ca | 116.7 (2) |
O5i—Mn—O8 | 103.60 (11) | C4—O4—Ca | 124.7 (2) |
O5—Mn—O8 | 87.46 (11) | C4—O5—Mn | 118.4 (2) |
O7i—Mn—O8i | 85.84 (12) | Ca—O6—H6A | 122.6 |
O7—Mn—O8i | 84.98 (11) | Ca—O6—H6B | 116.3 |
O5i—Mn—O8i | 87.46 (11) | H6A—O6—H6B | 100.3 |
O5—Mn—O8i | 103.60 (11) | Mn—O7—H7A | 118.9 |
O8—Mn—O8i | 165.58 (17) | Mn—O7—H7B | 129.9 |
O4ii—Ca—O4 | 141.27 (14) | H7A—O7—H7B | 104.8 |
O4ii—Ca—O6ii | 75.93 (9) | Mn—O8—H8A | 125.3 |
O4—Ca—O6ii | 79.93 (10) | Mn—O8—H8B | 119.5 |
O4ii—Ca—O6 | 79.93 (10) | H8A—O8—H8B | 109.5 |
O4—Ca—O6 | 75.93 (9) | H1A—O1W—H1B | 110.7 |
O6ii—Ca—O6 | 101.88 (13) | O1—C1—O2 | 126.0 (3) |
O4ii—Ca—O1ii | 126.00 (9) | O1—C1—C2 | 118.5 (3) |
O4—Ca—O1ii | 82.31 (10) | O2—C1—C2 | 115.6 (3) |
O6ii—Ca—O1ii | 157.90 (9) | O3—C2—C1 | 108.8 (3) |
O6—Ca—O1ii | 86.35 (9) | O3—C2—H2A | 109.9 |
O4ii—Ca—O1 | 82.31 (10) | C1—C2—H2A | 109.9 |
O4—Ca—O1 | 126.00 (9) | O3—C2—H2B | 109.9 |
O6ii—Ca—O1 | 86.35 (9) | C1—C2—H2B | 109.9 |
O6—Ca—O1 | 157.90 (9) | H2A—C2—H2B | 108.3 |
O1ii—Ca—O1 | 93.59 (13) | O3—C3—C4 | 107.7 (3) |
O4ii—Ca—O3ii | 63.95 (8) | O3—C3—H3A | 110.2 |
O4—Ca—O3ii | 142.07 (9) | C4—C3—H3A | 110.2 |
O6ii—Ca—O3ii | 137.09 (8) | O3—C3—H3B | 110.2 |
O6—Ca—O3ii | 86.09 (9) | C4—C3—H3B | 110.2 |
O1ii—Ca—O3ii | 63.19 (8) | H3A—C3—H3B | 108.5 |
O1—Ca—O3ii | 74.30 (9) | O4—C4—O5 | 124.1 (3) |
O4ii—Ca—O3 | 142.07 (9) | O4—C4—C3 | 119.3 (3) |
O4—Ca—O3 | 63.95 (8) | O5—C4—C3 | 116.6 (3) |
O6ii—Ca—O3 | 86.09 (9) |
Symmetry codes: (i) −x+1/2, −y+1/2, z; (ii) −x+3/2, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O1iii | 0.87 | 1.98 | 2.826 (4) | 163 |
O1W—H1B···O5 | 0.83 | 1.95 | 2.756 (4) | 166 |
O6—H6A···O2iv | 0.82 | 2.07 | 2.838 (4) | 156 |
O6—H6B···O1Wv | 0.85 | 1.92 | 2.772 (4) | 173 |
O7—H7A···O1Wiv | 0.88 | 1.97 | 2.751 (4) | 148 |
O7—H7B···O2vi | 0.97 | 1.84 | 2.797 (4) | 169 |
O8—H8A···O2vii | 0.92 | 1.92 | 2.838 (4) | 178 |
O8—H8B···O4i | 0.83 | 2.29 | 2.825 (4) | 122 |
O8—H8B···O6i | 0.83 | 2.31 | 3.094 (4) | 158 |
Symmetry codes: (i) −x+1/2, −y+1/2, z; (iii) x−1, y, z; (iv) x, −y+1/2, z+1/2; (v) x+1/2, y−1/2, −z+1; (vi) x−1, −y+1/2, z+1/2; (vii) −x+1, −y+1, −z+1. |