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The title compound, [Sr{Cl2C(PO3H)2}(H2O)5], is a monomer, the Sr atom being seven-coordinated by one chelating clodronate ligand and five aqua ligands. The coordination polyhedron can be described as a distorted monocapped trigonal prism. This compound is isostructural with hydrated calcium clodronate, [Ca{Cl2C(PO3H)2}(H2O)5], described previously [Nardelli, Pelizzi, Staibano & Zucchi (1983). Inorg. Chim. Acta, 80, 259-271].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015764/hg6061sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015764/hg6061Isup2.hkl
Contains datablock I

CCDC reference: 248713

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](P-C) = 0.004 Å
  • R factor = 0.019
  • wR factor = 0.047
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 100 PerFit PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... m PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Spacegroup . Pnma
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.504 From the CIF: _refine_ls_abs_structure_Flack_su 0.005 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.50 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT142_ALERT_4_C su on b - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl1 .. Cl2 .. 3.28 Ang.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.99 From the CIF: _reflns_number_total 2674 Count of symmetry unique reflns 1414 Completeness (_total/calc) 189.11% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1260 Fraction of Friedel pairs measured 0.891 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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.

Pentaaqua(dichloromethylenebisphosphonato)strontium(II) top
Crystal data top
[Sr(CH2Cl2O6P2)(H2O)5]F(000) = 832
Mr = 420.57Dx = 2.051 Mg m3
Dm = 2.02 (4) Mg m3
Dm measured by flotation
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 2674 reflections
a = 10.5207 (1) Åθ = 2.6–26.0°
b = 11.8587 (1) ŵ = 4.63 mm1
c = 10.9164 (2) ÅT = 120 K
V = 1361.95 (3) Å3Cubic, colourless
Z = 40.35 × 0.35 × 0.35 mm
Data collection top
Nonius KappaCCD
diffractometer
2674 independent reflections
Radiation source: fine-focus sealed tube2596 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
CCD scansθmax = 26.0°, θmin = 2.6°
Absorption correction: multi-scan
(XPREP in SHELXTL; Bruker, 1998)
h = 1212
Tmin = 0.182, Tmax = 0.198k = 1414
17202 measured reflectionsl = 1313
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-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 = 1.08Δρmax = 0.33 e Å3
2674 reflectionsΔρmin = 0.56 e Å3
156 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
1 restraintExtinction coefficient: 0.0028 (4)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 1260 Fiedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.504 (5)
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. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr0.014425 (17)0.569776 (14)0.39191 (3)0.00876 (7)
Cl10.24388 (6)0.31391 (4)0.40347 (9)0.02008 (14)
Cl20.51388 (6)0.37227 (5)0.40667 (9)0.02025 (17)
P10.32978 (8)0.51141 (7)0.54358 (6)0.00913 (17)
P20.33453 (9)0.50493 (6)0.25608 (7)0.00942 (18)
O10.1087 (2)0.67833 (14)0.22128 (17)0.0146 (4)
H1A0.18350.65770.20210.022*
H1B0.11420.74200.25670.022*
O20.15045 (19)0.68067 (16)0.51804 (18)0.0156 (4)
H2A0.11620.73870.54970.023*
H2B0.19920.65160.57150.023*
O30.0600 (3)0.41653 (19)0.5395 (2)0.0156 (5)
H3A0.12210.41740.58930.023*
H3B0.00640.39940.57970.023*
O40.0889 (3)0.4150 (2)0.2685 (2)0.0254 (7)
H4A0.11150.41960.19390.038*
H4B0.11830.35360.29700.038*
O50.10852 (14)0.76722 (11)0.3912 (2)0.0159 (3)
H5A0.18040.78590.42040.024*
H5B0.05840.82280.40060.024*
O110.1952 (2)0.55176 (18)0.5393 (2)0.0115 (5)
O120.4312 (2)0.6005 (2)0.54936 (19)0.0107 (5)
O130.3443 (3)0.42361 (17)0.6500 (2)0.0134 (5)
O210.2002 (2)0.54300 (19)0.2522 (2)0.0149 (5)
O230.3542 (3)0.41172 (18)0.1563 (2)0.0153 (5)
O220.4367 (2)0.59286 (19)0.25009 (18)0.0108 (5)
C10.3565 (2)0.42816 (15)0.4027 (4)0.0104 (5)
H130.43240.42010.66250.016*
H230.41580.40350.10660.016*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr0.00701 (11)0.01075 (10)0.00851 (11)0.00088 (6)0.00037 (15)0.00048 (13)
Cl10.0216 (3)0.0132 (2)0.0254 (3)0.00904 (19)0.0047 (4)0.0035 (4)
Cl20.0141 (3)0.0197 (3)0.0270 (5)0.00944 (19)0.0015 (4)0.0017 (4)
P10.0080 (4)0.0101 (4)0.0093 (4)0.0006 (3)0.0014 (3)0.0011 (3)
P20.0069 (4)0.0120 (4)0.0094 (4)0.0003 (3)0.0010 (3)0.0030 (3)
O10.0152 (11)0.0113 (8)0.0173 (9)0.0001 (7)0.0042 (8)0.0031 (8)
O20.0177 (11)0.0114 (9)0.0177 (10)0.0031 (8)0.0078 (8)0.0008 (7)
O30.0132 (12)0.0214 (12)0.0121 (10)0.0007 (9)0.0022 (9)0.0014 (8)
O40.0399 (18)0.0200 (12)0.0164 (11)0.0110 (10)0.0123 (11)0.0038 (9)
O50.0134 (7)0.0115 (6)0.0228 (8)0.0020 (6)0.0036 (12)0.0010 (11)
O110.0076 (12)0.0166 (11)0.0104 (10)0.0031 (9)0.0000 (9)0.0010 (8)
O120.0113 (12)0.0103 (10)0.0106 (10)0.0006 (9)0.0046 (9)0.0009 (8)
O130.0080 (11)0.0181 (11)0.0141 (11)0.0013 (8)0.0033 (8)0.0075 (8)
O210.0100 (13)0.0240 (12)0.0106 (11)0.0036 (10)0.0009 (9)0.0004 (9)
O230.0102 (12)0.0193 (11)0.0164 (11)0.0053 (9)0.0049 (8)0.0097 (9)
O220.0099 (12)0.0107 (10)0.0119 (10)0.0003 (8)0.0018 (9)0.0016 (8)
C10.0077 (10)0.0089 (9)0.0145 (12)0.0003 (7)0.0007 (14)0.0025 (12)
Geometric parameters (Å, º) top
Sr—O212.499 (2)P2—O231.566 (2)
Sr—O112.500 (2)P2—C11.856 (4)
Sr—O42.524 (2)O1—H1A0.8500
Sr—O52.542 (1)O1—H1B0.8500
Sr—O32.552 (2)O2—H2A0.8500
Sr—O22.576 (2)O2—H2B0.8500
Sr—O12.609 (2)O3—H3A0.8500
Cl1—C11.800 (2)O3—H3B0.8500
Cl2—C11.784 (2)O4—H4A0.8500
P1—O111.495 (3)O4—H4B0.8500
P1—O121.503 (3)O5—H5A0.8500
P1—O131.568 (2)O5—H5B0.8501
P1—C11.849 (4)O13—H130.9378
P2—O211.484 (2)O23—H230.8504
P2—O221.499 (3)
O21—Sr—O1177.69 (5)O22—P2—O23111.5 (1)
O21—Sr—O485.34 (8)O21—P2—C1107.0 (1)
O11—Sr—O4127.53 (8)O22—P2—C1106.8 (1)
O21—Sr—O579.08 (7)O23—P2—C1103.7 (1)
O11—Sr—O577.56 (7)Sr—O1—H1A119.5
O4—Sr—O5146.73 (8)Sr—O1—H1B98.5
O21—Sr—O3122.32 (8)H1A—O1—H1B107.7
O11—Sr—O376.49 (8)Sr—O2—H2A110.2
O4—Sr—O371.75 (7)Sr—O2—H2B124.5
O5—Sr—O3141.03 (8)H2A—O2—H2B107.7
O21—Sr—O2156.60 (7)Sr—O3—H3A129.1
O11—Sr—O2102.24 (7)Sr—O3—H3B104.1
O4—Sr—O2111.51 (8)H3A—O3—H3B107.7
O5—Sr—O278.09 (6)Sr—O4—H4A125.8
O3—Sr—O279.60 (7)Sr—O4—H4B125.7
O21—Sr—O190.88 (7)H4A—O4—H4B107.7
O11—Sr—O1151.57 (7)Sr—O5—H5A125.8
O4—Sr—O176.33 (7)Sr—O5—H5B118.2
O5—Sr—O174.73 (6)H5A—O5—H5B107.7
O3—Sr—O1130.53 (7)P1—O11—Sr140.2 (1)
O2—Sr—O178.19 (7)P1—O13—H13103.5
O11—P1—O12116.7 (1)P2—O21—Sr140.0 (1)
O11—P1—O13109.1 (1)P2—O23—H23128.7
O12—P1—O13111.5 (1)Cl2—C1—Cl1109.3 (1)
O11—P1—C1106.8 (1)Cl2—C1—P1108.6 (2)
O12—P1—C1107.6 (1)Cl1—C1—P1107.4 (2)
O13—P1—C1104.3 (1)Cl2—C1—P2108.6 (2)
O21—P2—O22118.0 (1)Cl1—C1—P2106.9 (2)
O21—P2—O23108.7 (1)P1—C1—P2115.9 (1)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O13i0.852.032.865 (3)168
O1—H1B···O22ii0.852.032.773 (3)145
O2—H2A···O12ii0.851.972.755 (3)153
O2—H2B···O23iii0.852.022.841 (3)162
O3—H3A···O21iii0.852.012.793 (3)152
O3—H3B···O1iii0.852.102.890 (3)155
O4—H4B···Cl1iv0.852.723.554 (3)167
O4—H4A···O11i0.851.932.768 (3)167
O5—H5A···O2v0.852.112.955 (3)171
O5—H5B···O12ii0.852.292.987 (3)139
O13—H13···O22vi0.941.682.558 (4)154
O23—H23···O12vii0.851.732.546 (3)161
Symmetry codes: (i) x, y+1, z1/2; (ii) x1/2, y+3/2, z; (iii) x, y+1, z+1/2; (iv) x1/2, 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, z1/2.
 

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