Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015764/hg6061sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015764/hg6061Isup2.hkl |
CCDC reference: 248713
Data collection: COLLECT (Nonius, 1997); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXL97.
[Sr(CH2Cl2O6P2)(H2O)5] | F(000) = 832 |
Mr = 420.57 | Dx = 2.051 Mg m−3 Dm = 2.02 (4) Mg m−3 Dm measured by flotation |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 2674 reflections |
a = 10.5207 (1) Å | θ = 2.6–26.0° |
b = 11.8587 (1) Å | µ = 4.63 mm−1 |
c = 10.9164 (2) Å | T = 120 K |
V = 1361.95 (3) Å3 | Cubic, colourless |
Z = 4 | 0.35 × 0.35 × 0.35 mm |
Nonius KappaCCD diffractometer | 2674 independent reflections |
Radiation source: fine-focus sealed tube | 2596 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
CCD scans | θmax = 26.0°, θmin = 2.6° |
Absorption correction: multi-scan (XPREP in SHELXTL; Bruker, 1998) | h = −12→12 |
Tmin = 0.182, Tmax = 0.198 | k = −14→14 |
17202 measured reflections | l = −13→13 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.019 | w = 1/[σ2(Fo2) + (0.02P)2 + 0.6P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.047 | (Δ/σ)max < 0.001 |
S = 1.08 | Δρmax = 0.33 e Å−3 |
2674 reflections | Δρmin = −0.56 e Å−3 |
156 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.0028 (4) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 1260 Fiedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.504 (5) |
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. There seems to be a pseudo centre of symmetry in the structure, and therefore the structure was solved as racemic twin. The solution in centrosymmetric space group Pnma was not satisfactory: the disorder increased and the R-factors did not decrease. |
x | y | z | Uiso*/Ueq | ||
Sr | 0.014425 (17) | 0.569776 (14) | 0.39191 (3) | 0.00876 (7) | |
Cl1 | 0.24388 (6) | 0.31391 (4) | 0.40347 (9) | 0.02008 (14) | |
Cl2 | 0.51388 (6) | 0.37227 (5) | 0.40667 (9) | 0.02025 (17) | |
P1 | 0.32978 (8) | 0.51141 (7) | 0.54358 (6) | 0.00913 (17) | |
P2 | 0.33453 (9) | 0.50493 (6) | 0.25608 (7) | 0.00942 (18) | |
O1 | −0.1087 (2) | 0.67833 (14) | 0.22128 (17) | 0.0146 (4) | |
H1A | −0.1835 | 0.6577 | 0.2021 | 0.022* | |
H1B | −0.1142 | 0.7420 | 0.2567 | 0.022* | |
O2 | −0.15045 (19) | 0.68067 (16) | 0.51804 (18) | 0.0156 (4) | |
H2A | −0.1162 | 0.7387 | 0.5497 | 0.023* | |
H2B | −0.1992 | 0.6516 | 0.5715 | 0.023* | |
O3 | −0.0600 (3) | 0.41653 (19) | 0.5395 (2) | 0.0156 (5) | |
H3A | −0.1221 | 0.4174 | 0.5893 | 0.023* | |
H3B | 0.0064 | 0.3994 | 0.5797 | 0.023* | |
O4 | −0.0889 (3) | 0.4150 (2) | 0.2685 (2) | 0.0254 (7) | |
H4A | −0.1115 | 0.4196 | 0.1939 | 0.038* | |
H4B | −0.1183 | 0.3536 | 0.2970 | 0.038* | |
O5 | 0.10852 (14) | 0.76722 (11) | 0.3912 (2) | 0.0159 (3) | |
H5A | 0.1804 | 0.7859 | 0.4204 | 0.024* | |
H5B | 0.0584 | 0.8228 | 0.4006 | 0.024* | |
O11 | 0.1952 (2) | 0.55176 (18) | 0.5393 (2) | 0.0115 (5) | |
O12 | 0.4312 (2) | 0.6005 (2) | 0.54936 (19) | 0.0107 (5) | |
O13 | 0.3443 (3) | 0.42361 (17) | 0.6500 (2) | 0.0134 (5) | |
O21 | 0.2002 (2) | 0.54300 (19) | 0.2522 (2) | 0.0149 (5) | |
O23 | 0.3542 (3) | 0.41172 (18) | 0.1563 (2) | 0.0153 (5) | |
O22 | 0.4367 (2) | 0.59286 (19) | 0.25009 (18) | 0.0108 (5) | |
C1 | 0.3565 (2) | 0.42816 (15) | 0.4027 (4) | 0.0104 (5) | |
H13 | 0.4324 | 0.4201 | 0.6625 | 0.016* | |
H23 | 0.4158 | 0.4035 | 0.1066 | 0.016* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sr | 0.00701 (11) | 0.01075 (10) | 0.00851 (11) | 0.00088 (6) | −0.00037 (15) | 0.00048 (13) |
Cl1 | 0.0216 (3) | 0.0132 (2) | 0.0254 (3) | −0.00904 (19) | 0.0047 (4) | −0.0035 (4) |
Cl2 | 0.0141 (3) | 0.0197 (3) | 0.0270 (5) | 0.00944 (19) | 0.0015 (4) | 0.0017 (4) |
P1 | 0.0080 (4) | 0.0101 (4) | 0.0093 (4) | −0.0006 (3) | −0.0014 (3) | 0.0011 (3) |
P2 | 0.0069 (4) | 0.0120 (4) | 0.0094 (4) | −0.0003 (3) | 0.0010 (3) | −0.0030 (3) |
O1 | 0.0152 (11) | 0.0113 (8) | 0.0173 (9) | −0.0001 (7) | −0.0042 (8) | −0.0031 (8) |
O2 | 0.0177 (11) | 0.0114 (9) | 0.0177 (10) | −0.0031 (8) | 0.0078 (8) | −0.0008 (7) |
O3 | 0.0132 (12) | 0.0214 (12) | 0.0121 (10) | −0.0007 (9) | 0.0022 (9) | 0.0014 (8) |
O4 | 0.0399 (18) | 0.0200 (12) | 0.0164 (11) | −0.0110 (10) | −0.0123 (11) | 0.0038 (9) |
O5 | 0.0134 (7) | 0.0115 (6) | 0.0228 (8) | 0.0020 (6) | −0.0036 (12) | −0.0010 (11) |
O11 | 0.0076 (12) | 0.0166 (11) | 0.0104 (10) | 0.0031 (9) | 0.0000 (9) | 0.0010 (8) |
O12 | 0.0113 (12) | 0.0103 (10) | 0.0106 (10) | −0.0006 (9) | −0.0046 (9) | −0.0009 (8) |
O13 | 0.0080 (11) | 0.0181 (11) | 0.0141 (11) | −0.0013 (8) | −0.0033 (8) | 0.0075 (8) |
O21 | 0.0100 (13) | 0.0240 (12) | 0.0106 (11) | 0.0036 (10) | 0.0009 (9) | 0.0004 (9) |
O23 | 0.0102 (12) | 0.0193 (11) | 0.0164 (11) | −0.0053 (9) | 0.0049 (8) | −0.0097 (9) |
O22 | 0.0099 (12) | 0.0107 (10) | 0.0119 (10) | 0.0003 (8) | 0.0018 (9) | −0.0016 (8) |
C1 | 0.0077 (10) | 0.0089 (9) | 0.0145 (12) | −0.0003 (7) | 0.0007 (14) | 0.0025 (12) |
Sr—O21 | 2.499 (2) | P2—O23 | 1.566 (2) |
Sr—O11 | 2.500 (2) | P2—C1 | 1.856 (4) |
Sr—O4 | 2.524 (2) | O1—H1A | 0.8500 |
Sr—O5 | 2.542 (1) | O1—H1B | 0.8500 |
Sr—O3 | 2.552 (2) | O2—H2A | 0.8500 |
Sr—O2 | 2.576 (2) | O2—H2B | 0.8500 |
Sr—O1 | 2.609 (2) | O3—H3A | 0.8500 |
Cl1—C1 | 1.800 (2) | O3—H3B | 0.8500 |
Cl2—C1 | 1.784 (2) | O4—H4A | 0.8500 |
P1—O11 | 1.495 (3) | O4—H4B | 0.8500 |
P1—O12 | 1.503 (3) | O5—H5A | 0.8500 |
P1—O13 | 1.568 (2) | O5—H5B | 0.8501 |
P1—C1 | 1.849 (4) | O13—H13 | 0.9378 |
P2—O21 | 1.484 (2) | O23—H23 | 0.8504 |
P2—O22 | 1.499 (3) | ||
O21—Sr—O11 | 77.69 (5) | O22—P2—O23 | 111.5 (1) |
O21—Sr—O4 | 85.34 (8) | O21—P2—C1 | 107.0 (1) |
O11—Sr—O4 | 127.53 (8) | O22—P2—C1 | 106.8 (1) |
O21—Sr—O5 | 79.08 (7) | O23—P2—C1 | 103.7 (1) |
O11—Sr—O5 | 77.56 (7) | Sr—O1—H1A | 119.5 |
O4—Sr—O5 | 146.73 (8) | Sr—O1—H1B | 98.5 |
O21—Sr—O3 | 122.32 (8) | H1A—O1—H1B | 107.7 |
O11—Sr—O3 | 76.49 (8) | Sr—O2—H2A | 110.2 |
O4—Sr—O3 | 71.75 (7) | Sr—O2—H2B | 124.5 |
O5—Sr—O3 | 141.03 (8) | H2A—O2—H2B | 107.7 |
O21—Sr—O2 | 156.60 (7) | Sr—O3—H3A | 129.1 |
O11—Sr—O2 | 102.24 (7) | Sr—O3—H3B | 104.1 |
O4—Sr—O2 | 111.51 (8) | H3A—O3—H3B | 107.7 |
O5—Sr—O2 | 78.09 (6) | Sr—O4—H4A | 125.8 |
O3—Sr—O2 | 79.60 (7) | Sr—O4—H4B | 125.7 |
O21—Sr—O1 | 90.88 (7) | H4A—O4—H4B | 107.7 |
O11—Sr—O1 | 151.57 (7) | Sr—O5—H5A | 125.8 |
O4—Sr—O1 | 76.33 (7) | Sr—O5—H5B | 118.2 |
O5—Sr—O1 | 74.73 (6) | H5A—O5—H5B | 107.7 |
O3—Sr—O1 | 130.53 (7) | P1—O11—Sr | 140.2 (1) |
O2—Sr—O1 | 78.19 (7) | P1—O13—H13 | 103.5 |
O11—P1—O12 | 116.7 (1) | P2—O21—Sr | 140.0 (1) |
O11—P1—O13 | 109.1 (1) | P2—O23—H23 | 128.7 |
O12—P1—O13 | 111.5 (1) | Cl2—C1—Cl1 | 109.3 (1) |
O11—P1—C1 | 106.8 (1) | Cl2—C1—P1 | 108.6 (2) |
O12—P1—C1 | 107.6 (1) | Cl1—C1—P1 | 107.4 (2) |
O13—P1—C1 | 104.3 (1) | Cl2—C1—P2 | 108.6 (2) |
O21—P2—O22 | 118.0 (1) | Cl1—C1—P2 | 106.9 (2) |
O21—P2—O23 | 108.7 (1) | P1—C1—P2 | 115.9 (1) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O13i | 0.85 | 2.03 | 2.865 (3) | 168 |
O1—H1B···O22ii | 0.85 | 2.03 | 2.773 (3) | 145 |
O2—H2A···O12ii | 0.85 | 1.97 | 2.755 (3) | 153 |
O2—H2B···O23iii | 0.85 | 2.02 | 2.841 (3) | 162 |
O3—H3A···O21iii | 0.85 | 2.01 | 2.793 (3) | 152 |
O3—H3B···O1iii | 0.85 | 2.10 | 2.890 (3) | 155 |
O4—H4B···Cl1iv | 0.85 | 2.72 | 3.554 (3) | 167 |
O4—H4A···O11i | 0.85 | 1.93 | 2.768 (3) | 167 |
O5—H5A···O2v | 0.85 | 2.11 | 2.955 (3) | 171 |
O5—H5B···O12ii | 0.85 | 2.29 | 2.987 (3) | 139 |
O13—H13···O22vi | 0.94 | 1.68 | 2.558 (4) | 154 |
O23—H23···O12vii | 0.85 | 1.73 | 2.546 (3) | 161 |
Symmetry codes: (i) −x, −y+1, z−1/2; (ii) x−1/2, −y+3/2, z; (iii) −x, −y+1, z+1/2; (iv) x−1/2, −y+1/2, z; (v) x+1/2, −y+3/2, z; (vi) −x+1, −y+1, z+1/2; (vii) −x+1, −y+1, z−1/2. |